Category: chlorides-buliding-blocks

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

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

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

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

Related Products of 4090-55-5, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 4090-55-5 name is 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

BODIE was obtained by the reaction of ethylenediamine with DOPC in trichloromethane.The DOPC (193.79 g, 1. 05 mol) and triethylamine (151.79 g, 1.5 mol)mixture with trichloromethane (200 mL) was put into a dry, four-necked flask equipped asdescribed above. The ethylenediamine (30 g, 0.5 mol) dissolved in trichloromethane(50 mL) was added dropwise at 0-5 C. After the addition, the temperature was increasedslowly to the reflux temperature and then the reaction was stopped after refluxing for 4 h.The resulting white precipitate was filtered and washed with cold distilled water and thendried overnight. The white product (BODIE) was obtained with a yield of 94 %. The massfraction purity of BODIE is 99 % measured by HPLC.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide, and friends who are interested can also refer to it.

Reference:
Article; Han, Feng; Pei, Liangjun; Xue, Fengfeng; Li, Dong; Journal of Solution Chemistry; vol. 45; 8; (2016); p. 1146 – 1157;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C8H7ClO2

Example 64: Synthesis of 3-(benzo[d][1 ,3]dioxol-5-ylmethyl)thiazolidine-2,4-dione; A suspension of thiazolidine-2,4-dione (10.0 mmol, 1.17 g), 5- (chloromethyl)benzo[d][1 ,3]dioxole (10.0 mmol, 50% soln in CH2CI2) and potassium fluoride (10.0 mmol, 0.581 g) is stirred at room temperature overnight. The solvent is removed under reduced pressure and the residue dissolved in H2O (50 ml_) and extracted into dichloromethane (3 x 20 ml_). Combined organic fractions were dried over Na2SO4 and the solvent removed under reduced pressure. The obtained oily product is washed with diethyl ether to give 1 .590 g (64%) of 3-(benzo[d][1 ,3]dioxol-5-ylmethyl)thiazolidine-2,4-dione as a white precipitate.

According to the analysis of related databases, 20850-43-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; LEK PHARMACEUTICAL D.D.; WO2008/43733; (2008); A1;,
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. 38762-41-3, name is 4-Bromo-2-chloroaniline, A new synthetic method of this compound is introduced below., Safety of 4-Bromo-2-chloroaniline

A degassed solution of l-methyl-3-(nonafluorobutane-l-sulfonyloxy)-lH- pyrrolo[3,2-c]pyridine-2-carboxylic acid ethyl ester (500 mg, 0.99 mmol), 4-bromo-2- chloroaniline (246 mg, 1.19 mmol), Pd2dba3 (91 mg, 0.10 mmol), Xantphos (114 mg, 0.20 mmol) and DBU (352 mul, 2.48 mmol) in toluene (8 ml) was subjected to microwave irradiation at 12OC for 5 minutes. The reaction mixture was cooled to ambient temperature then diluted with ethyl acetate (100 ml). The resultant solution was washed with water (30 ml), dried (Na2SO4) and concentrated in vacuo to give an oil. The oil was purified by flash chromatography (Si- PPC, cyclohexane: ethyl acetate, gradient 90:10 to 0:100) to afford the title compound as a yellow solid (140 mg, 35%). IH NMR (CDCl3, 400MHz) 8.75 (d, J = 1.0 Hz, IH), 8.41 (d, J = 6.1 Hz, IH), 7.68 (s, IH), 7.54 (d, J = 2.3 Hz, IH), 7.19-7.27 (m, 2H), 6.94 (d, J = 8.8 Hz, IH), 4.44 (q, J = 7.2 Hz, 2H), 3.99 (s, 3H), 1.44 (t, J = 7.2 Hz, 3H).

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; GENENTECH, INC.; WO2008/67481; (2008); A1;,
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. 102-49-8, name is 3,4-Dichlorobenzylamine, A new synthetic method of this compound is introduced below., HPLC of Formula: C7H7Cl2N

The product from the Example 20C (0.054 g, 0.20 mmol) in THF (3 mL) was stirred for 16 h at ambient temperature with 3,4-dichlorobenzylamine (0.044 g, 0.25 mmol) in the presence of triethylamine (0.35 mL, 0.25 mmol) and a catalytic amount of DMAP. The reaction mixture was evaporated in vacuo and the residue was chromatographed to yield the title compound as a solid. MS (DCI/NH3) m/z 406 (M+H)+; 1H NMR (DMSO-d6) delta 4.42 (d, 1H), 5.47 (s, 1H), 5.52 (d, 2H), 6.92 (dd, 1H), 7.31 (dd, 1H), 7.5 (d, 2H), 7.62 (m, 4H), 8.18 (s, 1H),8.82 (t, 1H).

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; Atkinson, Robert N.; Drizin, Irene; Gregg, Robert J.; Gross, Michael F.; Kort, Michael E.; Shi, Lei; US2004/220170; (2004); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 4152-90-3, A common heterocyclic compound, 4152-90-3, name is (3-Chlorophenyl)methanamine, molecular formula is C7H8ClN, 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.

3- [5,6-bis(methyloxy)-2-pyridinyll -N- [(3-chlorophenvDmethyll -2,4-dioxo-l ,2,3,4-tetrahvdro- 7-quinazolinecarboxamide; 24a) Methyl 2-amino-4-(3-chlorobenzylaminocarbonyl)benzoate; To a stirred suspension of 3-amino-4-(methoxycarbonyl)benzoic acid (1.0 g, 5.13 mmol, 1 eq.) in DMF (7 mL) was added HATU (2.1 g, 0.5.64 mmol, 1.1 eq.) and DIEA (0.98 mL, 0.11 mol, 1.1 eq.) and the mixture was stirred at rt for 5 minutes until all dissolved. The resulting solution was added to 3-chlorobenzylamine (0.69 mL, 5.64 mmol, 1.1 eq.) in DMF (3 mL) via syringe and stirred at rt for 30 minutes when LCMS showed that the reaction was complete. The solution was added dropwise to ice-water with stirring and the precipitate collected by vacuum filtration, washed with ice-water and dried under vacuum to yield the title product methyl 2-amino-4-(3 chlorobenzylaminocarbonyl)benzoate (24a) which was used without further purification. (Yield: 1.52g, 93percent); MS(ES+) m/e 319 (MH+); 1H NMR (400 MHz, OMSO-d6) delta ppm: 3.81 (s, 3 H) 4.44 (d, J 6.06 Hz, 2 H) 6.81 (s, 2 H) 6.97 (d, J 8.59 Hz, 1 H) 7.24 – 7.40 (m, 5 H) 7.77 (d, J 8.59 Hz, 1 H) 9.07 (t, J 6.06 Hz, 1 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; GLAXOSMITHKLINE LLC; SCHULZ, Mark, James; WANG, Yonghui; WO2010/59549; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 104-11-0, name is 1-(4-Chlorophenyl)-N-methylmethanamine, 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 104-11-0, name: 1-(4-Chlorophenyl)-N-methylmethanamine

General procedure: An amine (1 mmol, 2 equiv) was added to a solution of Nchlorosuccinimide(149 mg, 1.1 mmol, 2.2 equiv) in CH2Cl2(5 mL) at r.t. in the dark. After 3 h, Ir(dtbpy)(ppy)2PF6 (4 mg,5 mumol, 0.01 equiv), Ph3N (245 mg, 1 mmol, 2 equiv), andbenzoxazole (60 mg, 0.5 mmol, 1 equiv) were added. Thereaction rube was sealed and placed at a distance of 5 cm from 3 W blue LED and stirred for 60 h. After the reactionwas complete, the solvent was evaporated under vacuo. Thecrude mixture was purified by flash column chromatographyeluting with a mixture of PE-EtOAc. 2-(4-Morpholinyl)benzoxazole (3a)Known compound; yellow solid; mp 85-87 C. 1H NMR(400 MHz, CDCl3): delta = 7.37 (d, J = 7.6 Hz, 1 H), 7.27 (d,J = 6.4 Hz, 1 H), 7.18 (t, J = 7.6 Hz, 1 H), 7.04 (t, J = 7.6 Hz,1 H), 3.82 (t, J = 4.4 Hz, 4 H), 3.69 (t, J = 5.2 Hz, 4 H). 13CNMR (100 MHz, CDCl3): delta = 162.0, 148.7, 142.8, 124.0,120.9, 116.4, 108.8, 66.1, 45.7.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Article; Wang, Jia-Di; Liu, Yu-Xia; Xue, Dong; Wang, Chao; Xiao, Jianliang; Synlett; vol. 25; 14; (2014); p. 2013 – 2018;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics