Category: chlorides-buliding-blocks

Electric Literature of 14862-52-3, These common heterocyclic compound, 14862-52-3, name is 3,5-Dibromochlorobenzene, 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.

Potassium phosphate mono-hydrate (K3PO4.H2O, 8 g, 40 mmol, 2 equiv) and 1-chloro-3,5-dibromobenzene (2.4 g, 8.93 mmol) were added into the reaction solution of EXAMPLE 2, then refluxed at 110 C. overnight under argon atmosphere. Then cooled to ambient temperature. Distilled water (30 mL) was added via a funnel, and the resulting mixture was filtered on a Buechner funnel. The filtrate was transferred to a separatory funnel and extracted with CH2Cl2 (3¡Á50 mL). The combined organic phases were dried over Na2SO4, filtered on filter paper and concentrated to dryness by rotary evaporation (30 C., 25 mmHg). The resulting yellow solid was purified by column chromatography to afford 3.33 g white solid (90%). Compound G: 1H NMR (400 MHz, CDCl3). 8.97 (s, 2H), 8.67 (d, 2H), 8.08 (d, 2H), 7.84 (s, 2H), 7.76(s,1H), 7.73-7.71(m, 2H), 7.66-7.63 (m, 6H), 7.54-7.50 (m, 2H).

Statistics shows that 3,5-Dibromochlorobenzene is playing an increasingly important role. we look forward to future research findings about 14862-52-3.

Reference:
Patent; General Electric Company; US2010/331547; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 4584-46-7, These common heterocyclic compound, 4584-46-7, name is 2-Chloro-N,N-dimethylethanamine hydrochloride, 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.

A flame-dried two-necked 25 mL round-bottomed flask was charged with cyclic sulfite (1 mmol), Fe3+-clay (100 mg) and dry xylene (5 mL) and stirred under a constant flush of nitrogen. Freshly distilled 2-aminothiophenol (0.9 mmol) was added drop wise, and the reaction mixture was refluxed for 12 h. Crude compound was chromatographed to get cis-(+)-2,3-dihydro-3-hydroxy-2-(4-methoxyphenyl)-1,5-benzothiazepin-4(5H)-one (50% yield). The hydroxy lactam (0.54 mmol) was dissolved in ethyl acetate (5 mL) and 2-(dimethylamino) ethyl chloride hydrochloride (0.694 mmol) was added followed by addition of finely ground K2CO3 (2.16 mmol) and a drop of water. The heterogeneous mixture was stirred at reflux for 12 h. Solvent was removed and the crude product was chromatographed to obtain N-alkylated product (88%).

The synthetic route of 4584-46-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; COUNCIL OF SCIENTIFIC AND INDUSTRIAL RESEARCH; WO2004/58734; (2004); 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. 13726-14-2, name is 4-Chloro-3-methoxyaniline, A new synthetic method of this compound is introduced below., SDS of cas: 13726-14-2

A mixture of 26 (0.25 mmol), 3-chloro-4-methoxyaniline (0.75 mmol), TEA (0.75 mmol) and NaI (0.025 mmol) in NMP (2 mL) was heated to 130 C. and stirred overnight. The mixture was diluted with AcOEt (10 mL) and washed with H2O (2¡Á10 mL). The organic layers were dried over Na2SO4, filtered and evaporated under reduce pressure. Flash Chromatography (eluent: 5% MeOH in AcOEt) gave the desired product L (10% yield). MS ESI (m/z) 407 (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; THE TRUSTEES OF COLUMBIA UNIVERSITY IN THE CITY OF NEW YORK; Landry, Donald W.; Deng, Shixian; Arancio, Ottavio; Fiorito, Jole; Wasmuth, Andrew; (41 pag.)US10626113; (2020); B2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 328-84-7, These common heterocyclic compound, 328-84-7, name is 3,4-Dichlorobenzotrifluoride, 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.

Example 15 Preparation of Compound No. 77 To a solution of 5-nitroindazole in N,N-dimethylformamide (20 g), 60% sodium hydride (0.5 g) was added slowly, and the resultant mixture was stirred while cooling with ice for 30 minutes. To the mixture, 3,4-dichlorobenztrifluoride (2.2 g) was added, and the resultant mixture was stirred at 80 C. for 2 hours. After completion of the reaction, the reaction mixture was poured into water and extracted with ethyl acetate. The extract was concentrated and the residue was purified by silica gel column chromatography with hexane-ethyl acetate (4:1) to give 1-(2-chloro-4-trifluoromethylphenyl)-5-nitroindazole (2.1 g).

The synthetic route of 328-84-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sumitomo Chemical Company, Limited; US5266556; (1993); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 33786-89-9, 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. 33786-89-9, name is 5-Chloro-m-phenylenediamine, This compound has unique chemical properties. The synthetic route is as follows.

REFERENCE EXAMPLE 75 To a solution of 5-chloro-1,3-benzenediamine (7.48 g) in tetrahydrofuran (50 ml) was added slowly a 1.5M solution of n-butyl lithium in n-hexane (27.3 ml) at 0 C. The resultant mixture was stirred for 30 minutes at 0 C. To the mixture was added a solution of 3-chloro-6-fluorobenzo[d]isoxazole (1.8 g) in tetrahydrofuran (5 ml). After stirring for 15 minutes at 0 C. and for an hour at ambient temperature, the reaction mixture was poured into a mixture of water and ethyl acetate. The separated organic layer was washed well with 1N-hydrochloric acid and dried over potassium carbonate. After evaporation under reduced pressure, the residue was crystallized from methanol to give 5-chloro-N-(6-fluorobenzo[d]isoxazol-3-yl)benzene-1,3-diamine (1.54 g). APCI-Mass: 278 (m/z, (M+H)+) NMR(DMSO-d6, delta): 5.50(2H, s), 6.24(1H, t, J=3.7 Hz), 6.88(2H, t, J=1.9 Hz), 7.27(1H, dt, J=2.1, 9.0 Hz), 7.57(1H, dd, J=2.1, 9.0 Hz), 8.09-8.22(1H, m), 9.47(1H, s).

The chemical industry reduces the impact on the environment during synthesis 5-Chloro-m-phenylenediamine. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Yamada, Akira; Spears, Glen; Hayashida, Hisashi; Tomishima, Masaki; Ito, Kiyotaka; Imanishi, Masashi; US2003/176454; (2003); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

7006-52-2, name is N-Methyl-3-chloroaniline, belongs to chlorides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Computed Properties of C7H8ClN

TBAI in the reaction bottle (0.3mmol, 111 mg), compound1j (2mmol, 282 mg), compound2 (4mmol, 341 mg), NaOAc (4mmol, 164 mg), TBHP (0.60 ml), water (4.0 ml), tetrahydrofuran (4.0 ml). Then the system in the air 80 ¡ãC heating under the conditions of about 12 hours, quenched with saturated sodium sulfite solution, extraction with ethyl acetate (40 ml ¡Á 3), silica gel adsorption, through the simple column chromatography can get product3j,the yield is 75percent. The prepared test data mainly of the product are as follows, can be known through the analysis, the actual synthetic product is consistent with the theoretical analysis.

The synthetic route of 7006-52-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Suzhou University; Wan, Xiaobing; Wang, Hongxiang; Zhang, Jie; Shao, Ying; (22 pag.)CN105237435; (2016); A;,
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. 94-97-3, name is 5-Chloro-1H-benzo[d][1,2,3]triazole, This compound has unique chemical properties. The synthetic route is as follows., Safety of 5-Chloro-1H-benzo[d][1,2,3]triazole

General procedure: 1-phenylbutane-1,3-dione 1a (0.2 mmol, 32.4 mg), 1H-benzo[d][1,2,3]triazole 2a (0.2 mmol, 23.8 mg), N-bromosuccinimide (NBS) (39.2 mg, 1.2 equiv), KOtBu (44.8 mg, 2 equiv) and EtOAc (2 mL) were added to a flask with a magnetic stirring bar. The resulting mixture was stirred for 6 h at 60 oC. After cooling to room temperature, the mixture was diluted with ethyl acetate and filtered. The filtrate was removed under reduced pressure to get the crude product, which was further purified by silica gel chromatography (petroleum/ethyl acetate = 5/1-2/1 as eluent) to give product 3a and 4a as light yellow and pink solids. The identity and purity of the products was confirmed by 1H and 13C NMR spectroscopic analysis

According to the analysis of related databases, 94-97-3, the application of this compound in the production field has become more and more popular.

Reference:
Article; Chen, Wen-Lin; Li, Ji-Hui; Meng, Xu; Tang, Dong; Guo, Shuai-Bo; Chen, Bao-Hua; Tetrahedron Letters; vol. 54; 4; (2013); p. 295 – 299;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 24279-39-8, These common heterocyclic compound, 24279-39-8, name is 2,6-Dichloro-4-(trifluoromethyl)aniline, 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.

CuBr2 (4.02 g, 18.0 mmol) and tert-butyl nitrite (3.12 g, 30.3 mmol)were added together with MeCN (60 mL) to a three-necked flask underargon. In a separate flask, 2,6-dichloro-4-trifluoromethylaniline(3.5 g, 15.2 mmol) was dissolved in MeCN (20 mL) under argon. Theaniline solution was then added dropwise to the three-necked flaskcontaining the nitrite mixture. The reaction mixture was then heatedto 65 C and stirred overnight. The mixture was cooled to r.t. andpoured into a separatory funnel with H2O (50 mL) and Et2O (110 mL).The organic layer was separated and washed with aq 3 M HCl (2 ¡Á 30mL). The organic layer was dried (Na2SO4), concentrated by rotaryevaporation and high vacuum to completely remove the volatiles;yield: 3.79 g (85%); colorless oil.1H NMR (300 MHz, CDCl3): delta = 7.63 (s, 2 H).13C NMR (100 MHz, CDCl3): delta = 137.4, 131.1 (q, J = 34 Hz), 127.9, 125.2(q, J = 3.1 Hz), 122.4 (q, J = 271 Hz).

Statistics shows that 2,6-Dichloro-4-(trifluoromethyl)aniline is playing an increasingly important role. we look forward to future research findings about 24279-39-8.

Reference:
Article; Miller, Daniel K.; Bailey, Christopher A.; Sammelson, Robert E.; Synthesis; vol. 47; 18; (2015); p. 2791 – 2798;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

6579-54-0, name is 2,6-Dichlorobenzenesulfonyl chloride, belongs to chlorides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. HPLC of Formula: C6H3Cl3O2S

2,6-Dichloro-3-nitrobenzenesulfonic acid Lithium hydroxide hydrate (8.96 g, 0.214 mol) was added to a solution of 2,6-dichlorobenzenesulfonyl chloride (35 g, 0.146 mol) in MeOH (300 mL) and the reaction was allowed to stir at room temperature for 16 hr. The reaction mixture was filtered to remove suspended solids and then concentrated. The resulting solid was dried in vacuo overnight to remove any residual MeOH. The solid was then dissolved in H2SO4 (300 mL) and chilled in an ice bath. A solution of H2SO4 (35 mL) and HNO3 (70%, 10.7 mL) was slowly added to the above reaction over 90 min. The reaction was allowed to warm up to room temperature overnight and then slowly poured into ice water (1200 mL) and extracted with EtOAc. The combined organic layers were dried (MgSO4) and concentrated to yield 2,6-dichloro-3-nitrobenzenesulfonic acid (37.38 g, 96%) as the dihydrate. EI-MS (m/z) 270 (M-).

The synthetic route of 6579-54-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Palovich, Michael R; Widdowson, Katherine L; Nie, Hong; US2003/50298; (2003); 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. 3386-33-2, name is 1-Chlorooctadecane, A new synthetic method of this compound is introduced below., Quality Control of 1-Chlorooctadecane

REFERENCE EXAMPLE 30 Preparation of (1R,2R)-2-(Stearoylamino)cyclohexanol (1R,2R)-2-Aminocyclohexanol (1.15 g) and 3.02 g of stearyl chloride were reacted in the same manner as in Reference Example 20 to obtain 3.0 g of the objective compound (yield: 100%). Property: Oily. Mass Spectrometric Analysis: Molecular formula: C24 H47 NO2, Calculated: 381.3606, Found: 381.3611. NMR(delta, CDCl3): 0.88 (3H,t,J=7Hz), 1.11-1.41 (32H,m), 1.57-1.78 (4H,m), 1.89-2.11 (2H,m), 2.22 (2H,t,J=7Hz), 3.31 (1H,ddd,J=11Hz,11Hz, 5Hz), 3.58-3.70 (1H,m), 5.42-5.51 (1H,m).

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; Fujirebio Inc.; US5120738; (1992); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics