Chlorides-buliding-blocks

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 622-86-6 as follows. Safety of (2-Chloroethoxy)benzene

a. Diethyl 2,2-di(2-phenoxyethyl)malonate To a stirred solution of sodium (2.3 g) in absolute EtOH (50 ml) was added diethyl malonate (15.2 ml) followed by 2-phenoxyethyl chloride (15. 7 g). The reaction mixture was then refluxed for 12 hr. The EtOH was evaporated under vacuum and the mixture diluted with water (40 ml). The aqueous phase was extracted with Et2 O. The combined Et2 O extracts were washed (brine), dried (MgSO4) filtered and evaporated. Bulb to bulb distillation afforded 12.2 g (27%) of the title diester as a clear liquid, bp 155-175 (106 Pascals, 0.8 Torr); TLC, Rf =0.34, CH2 Cl2.

According to the analysis of related databases, 622-86-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ICI Americas Inc.; US4910190; (1990); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 50638-46-5,Some common heterocyclic compound, 50638-46-5, name is 4-Bromo-3-chloroanisole, molecular formula is C7H6BrClO, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Step 1: Preparation of 4-hydroxy-1-(2-chloro-4-methoxyphenyl)-2-methylbutan-1-one [0064] To a 1.0 L, 3-neck round bottom flask, equipped with a mechanical stirrer and an internal thermometer, was added a solution of 4-bromo-3-chloroanisole (12.0 g, 54.0 mmol) in 350 mL of THF under nitrogen. The solution was cooled to -85 C. with a MeOH/liquid nitrogen bath. To this solution was added t-BuLi (72.0 mL, 1.6 M in pentane, 122 mmol) slowly followed by the addition of a solution of alpha-methyl-gamma-butyrolactone (9.25 g, 92.0 mmol) in THF (30.0 mL). The internal temperature was controlled <-80 C. After 1 h stirring at <-80 C., the reaction mixture was quenched with saturated NH4Cl solution and warmed to room temperature. Water and EtOAc were added and separated. The aqueous layer was extracted with EtOAc (2×). The combined organic solutions was dried (MgSO4) and filtered. The filtrate was concentrated in vacuo to dryness. The residue was subjected to column chromatography (E:H, 1:3) to give 10.4 g (79%) of brown oil as the title compound: 1H NMR (400 MHz, CDCl3) delta 7.53 (d, J =8.6 Hz, 1H), 6.97 (d, J =2.4 Hz, 1H), 6.85 (dd, J =8.6, 2.4 Hz, 1H), 3.88 (s, 3H), 3.77-3.69 (m, 2H), 3.64-3.56 (m, 1H), 2.16-2.07 (m, 1H), 1.76-1.67 (m, 1H), 1.23 (d, J=7.0 Hz, 3H); MS (El m/z 241.16 (M+-H). These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4-Bromo-3-chloroanisole, its application will become more common. Reference:
Patent; Pfizer Inc; US2004/204415; (2004); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some common heterocyclic compound, 6276-54-6, name is 3-Chloropropan-1-amine hydrochloride, molecular formula is C3H9Cl2N, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. category: chlorides-buliding-blocks

Triethylamine (51.0 g) was added dropwise to a solution of di-tert-butyl dicarbonate (100.0 g) and 3-chloropropylamine hydrochloride (71.5 g) in methanol (400 mL) at 0 C., and the mixture was then stirred at the same temperature for 16 hours. Thereafter, toluene (400 mL) and water (400 mL) were added to the reaction solution for liquid separation, and the organic layer was then washed with water. 400 mL of toluene was added to the organic layer, and the mixed solution was concentrated to 300 mL under reduced pressure. After that, N,N-dimethylacetamide (210 mL) was added, and the mixed solution was concentrated to 300 mL under reduced pressure. Thereafter, to this solution, potassium carbonate (126.66 g), tetrabutylammonium bromide (44.32 g), dimethyl malonate (90.82 g) and N,N-dimethylacetamide (100 mL) were added, and the mixed solution was then stirred at 55 C. for 20 hours. Thereafter, toluene (400 mL) and water (700 mL) were added to the reaction solution for liquid separation. The organic layer was successively washed with water, a 1 M aqueous sodium hydroxide solution and water, and was then concentrated to 150 mL under reduced pressure. To this solution, methanol (1870 mL) and a 1 M aqueous sodium hydroxide solution (430.8 mL) were added, and the mixed solution was then stirred at 0 C. for 27.5 hours. Subsequently, concentrated hydrochloric acid (2.5 mL) was added to the reaction solution, so that the pH of the solution was adjusted to pH 7-9, and the solution was then concentrated to 375 mL under reduced pressure. Ethyl acetate (500 mL) was added to the reaction solution, and concentrated hydrochloric acid (35.1 mL) was then added to the mixed solution, so that the pH of the solution was adjusted to pH 2.2-2.5, followed by liquid separation. The water layer was extracted with ethyl acetate (500 mL), the organic layer was then mixed therewith. The mixed solution was dehydrated and concentrated under reduced pressure to prepare an ethyl acetate (250 mL) solution. To the obtained solution, ethyl acetate (500 mL) and morpholine (37.5 g) were added, and the obtained mixture was stirred overnight. Thereafter, the precipitated crystals were filtrated, were then washed with ethyl acetate, and were then dried under reduced pressure to obtain the title compound (136.1 g, yield: 81.9%). (0118) 1H-NMR (DMSO-d6) delta: 6.79 (1H, t, J=5.5 Hz), 3.61 (4H, t, J=4.9 Hz), 3.58 (3H, s), 3.14 (1H, t, J=7.8 Hz), 2.90-2.80 (6H, m), 1.74-1.59 (2H, m), 1.37 (9H, s), 1.34-1.25 (2H, m) .

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 6276-54-6, its application will become more common.

Reference:
Patent; DAIICHI SANKYO COMPANY, LIMITED; HAYASHI, Masaki; UKAI, Kazutoshi; (16 pag.)US2018/29993; (2018); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 53145-38-3, name is 2-Chloro-6-fluoroanisole, belongs to chlorides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 53145-38-3, Computed Properties of C7H6ClFO

The product of preparation 20 (150mg, 0.431 mmol) in dimethylformamide (3ml) was added drop wise to an ice-cooled solution of sodium hydride (60% dispersion in mineral oil, 52mg,1.293mmol) in dimethylformamide (1ml). After stirring for 1 hour the product of preparation 22(103mg, 0.646mmol) in dimethylformamide (1ml) was added and the mixture was heated to60c for 96 hours. The solution was concentrated in vacuo and partitioned between ethyl acetate (10ml) and water (10ml). The organic layer was extracted and washed again with water (10ml), then dried over sodium sulphate and concentrated in vacuo, to afford the title compound as a brown oil in 74% yield, 156mg.1HNMR(400MHz, CD3OD) delta: 1.03(s, 3H), 1.08(s, 3H), 1.44-1.49(m, 2H), 1.90-1.97(m, 1H), 2.12-2.21 (m, 1H), 2.50-2.62(m, 3H), 2.74-2.83(m, 2H), 2.87-2.91 (m, 1H), 3.74(s, 3H), 4.81- 4.84(m, 1H), 6.83-6.85(dd, 1H), 6.93-7 ,00(m, 2H), 7.25-7.42(m, 10H); LRMS ESI m/z 489 [M+H]+

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Chloro-6-fluoroanisole, and friends who are interested can also refer to it.

Reference:
Patent; PFIZER LIMITED; WO2007/34325; (2007); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some common heterocyclic compound, 870-24-6, name is 2-Chloroethanamine hydrochloride, molecular formula is C2H7Cl2N, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Application In Synthesis of 2-Chloroethanamine hydrochloride

In a round-bottomed flask, 2-chloroethylamine hydrochloride (2 g, 17.0 mmol) and Et3N (2.37 mL, 11.0 mmol) were dissolved in anhydrous CH2Cl2 (24 mL). Boc2O (3.6 mL, 15.3 mmol) was added to the resulting solution under N2 at 0 C. The reaction mixture was stirredat r.t. for 4 h. The mixture was then washed with H2O and brine, dried (Na2SO4), filtered, and concentrated under reduced pressure to give the title product as a dark liquid; yield: 2.91 g (16.21 mmol, 99%), which was used directly in the next synthetic step. IR (neat): 3347, 2924, 2854, 2361, 2342, 1725, 1709, 1503, 1462 cm-1. 1H NMR (400 MHz, CDCl3): delta = 1.18 [s, 9 H, C(CH3)3], 3.36-3.48 (m, 2H, CH2NH), 3.49-3.63 (m, 2 H, ClCH2), 4.93 (br s, 1 H, NHCO). 13C NMR (100 MHz, CDCl3): delta = 28.2 [C(CH3)3], 32.8 (CH2NH), 45.7 (CH2Cl), 79.8 [C(CH3)3], 155.8 (C=O). Anal. Calcd for C7H14ClNO2: C, 46.80; H, 7.86; N, 7.80. Found: C, 46.91; H, 7.89; N, 7.74.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 870-24-6, its application will become more common.

Reference:
Article; Manasieva, Leda Ivanova; Maria, Battisti Umberto; Prandi, Adolfo; Brasili, Livio; Franchini, Silvia; Synthesis; vol. 47; 23; (2015); p. 3767 – 3775;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 1996-29-8, name is 1-Bromo-4-chloro-2-fluorobenzene, A new synthetic method of this compound is introduced below., Recommanded Product: 1996-29-8

General Procedure: In a 2OmL tube equipped with a stir bar added l-bromo-4-chloro-2- fluorobenzene (Ig, 4.77mmol), ‘butyl- 1-piperazinecarboxylate (1.74g, 9.55mmol), palladium acetate (0.107g, 0.48mmol), 2-ditbutylphosphenylbiphenyl (0.143g, 0.48mmol), sodium tert- butoxide (0.688g, 7.16mmol) and toluene (10 mL). The reaction vessel was sealed and placed in a microwave oven at 15O0C for 15 min. The reaction mixture was filtered though Diatomaceous earth. The filtrate was diluted with ethyl acetate (50 mL), sequentially washed with water (3 x 5OmL) and brine (5OmL) in a separation funnel. The organic layer was dried over anhydrous sodium sulfate, filtered and concentrated in vacuo. The crude residue was purified on silica gel using hexanes: ethyl acetate= 93: 7 to hexanes: ethyl acetate= 95: 5 in a gradient fashion, to isolate the desired product as yellow oil (639mg, 43%). 1H NMR (300 MHz, CDCl3): delta 7.03 (m, 2H), 6.83(m, IH), 3.57 (t, 4H)5 2.95 (t, 4H), 1.46 (s, 9H).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; ASTRAZENECA AB; NPS PHARMACEUTICALS, INC.; WO2007/87135; (2007); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 328-84-7, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 328-84-7, name is 3,4-Dichlorobenzotrifluoride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

The procedure of Example 4 was repeated but using 3,4-dichlorobenzotrifluoride. After work up there was isolated a 95% yield of the title compound. It was shown that 100% of the starting material had been consumed, thus indicating that the reaction had occurred with both high selectivity and high yield. The above reaction was repeated but using various other solvents. The following yields of title compound were obtained: tetrahydrofuran 90 1,4-dioxan 93 N,N,N’,N’-tetramethylurea 72

The synthetic route of 3,4-Dichlorobenzotrifluoride has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Aventis CropScience, S.A.; US6410737; (2002); B1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some common heterocyclic compound, 61881-19-4, name is 2,2,2-Trifluoro-N-phenylacetimidoyl chloride, molecular formula is C8H5ClF3N, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Product Details of 61881-19-4

General procedure: A mixture of acetimidoyl chloride (1 mmol), sodium azide (1 mmol), and acetonitrile (3 mL) was irradiated in a microwave oven at 300 W for 8-10 min, after completion of the reaction, as indicated by TLC, the reaction mixture was filtered. After removing the solvent under reduced pressure, if necessary, the crude products were purified by washing with n-hexane to give the target product 3a-3j (90-95%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 61881-19-4, its application will become more common.

Reference:
Article; Rahmani, Fariba; Darehkordi, Ali; Notash, Behrouz; Journal of Fluorine Chemistry; vol. 166; (2014); p. 84 – 87;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 63624-28-2, name is 2,4-Dimethoxybenzene-1-sulfonyl chloride, A new synthetic method of this compound is introduced below., Formula: C8H9ClO4S

A solution of 2,4-dimethoxybenzene-1-sulfonyl chloride (0.0799 g, 0.337 mmol) and 5-methylbenzo[d]isoxazol-3-amine I60 (0.050 g, 0.34 mmol) in pyridine (1 ml.) was irradiated in the microwave at 110 C for 2 hours. The resultant mixture was loaded onto silica gel and the product purified by column chromatography (12 g S1O2 cartridge, 0-45% EtOAc in petroleum benzine 40-60 C) [205] to yield the title compound (55.0 mg, 42% yield) as a white solid. NMR (400 MHz, CDCb) d 7.86 – 7.82 (m,1H), 7.72 (d, J = 8.81Hz, 1H), 7.37 – 7.28 (m, 2H), 6.49 (d, J = 2.26 Hz, 1H), 6.43 (dd, J = 2.29, 8.82 Hz, 1H), 3.96 (s, 3H), 3.80 (s, 3H), 2.47 (s, 3H). LCMS-A: rt 5.66 min, m/z 348.8 [M+H]+, 347.1 [M-H]

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; CTXT PTY LIMITED; STUPPLE, Paul, Anthony; LAGIAKOS, Helen, Rachel; MORROW, Benjamin, Joseph; FOITZIK, Richard, Charles; HEMLEY, Catherine, Fae; CAMERINO, Michelle, Ang; BOZIKIS, Ylva, Elisabet, Bergman; WALKER, Scott, Raymond; (321 pag.)WO2019/243491; (2019); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 60811-21-4, name is 4-Bromo-2-chloro-1-fluorobenzene, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Recommanded Product: 4-Bromo-2-chloro-1-fluorobenzene

4-Bromo-2-chloro-l- fluorobenzene (1; 16 g, 76.5 mmol) was dissolved in 50 mL of THF. The reaction mixture was cooled down to -78 C. A solution of LDA in THF (2 M, 38.2 mL, 76.4 mmol) was added dropwise over 20 min. The reaction mixture was stirred at -78 C for 10 min. DMF (8.4 mL) was added dropwise. The reaction mixture was allowed to warm -20 C and quenched with 30 mL of saturated ammonium chloride aqueous solution, extracted with methyl tert- at l ether (50 mL X 3). The combined organic layers were washed with brine, dried over anhydrous Na2S04, and concentrated under reduced pressure to give crude product, which was purified by silica gel chromatography (5-10% EtO Ac/petroleum ether) to afford 8.4 g of 5-bromo-3-chloro-2-fluorobenzaldehyde (2) as white solid (yield: 46%). 1H MR (400 MHz, DMSO-i) delta 10.10 (s, 1H), 8.26 (s, 1H), 7.93 (s, 1H).

The synthetic route of 4-Bromo-2-chloro-1-fluorobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; KARYOPHARM THERAPEUTICS INC.; BALOGLU, Erkan; SENAPEDIS, William; SHACHAM, Sharon; (160 pag.)WO2016/100515; (2016); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics