Category: chlorides-buliding-blocks

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. 2106-02-7, name is 2-Chloro-4-fluoroaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Safety of 2-Chloro-4-fluoroaniline

To a solution of 197 mg (1.35 mmol) of 2-chloro-4-fluoroaniline and 0.20 ml (1.42 mmol) of triethylamine in 5 ml of ethyl acetate was added dropwise a solution of 400 mg (1.29 mmol) of ethyl 8-chlorosulfonyl-1,4-dioxaspiro[4.5]dec-7-ene-7-carboxylate obtained in (1c) in 3 ml of ethyl acetate with stirring under ice-cooling, followed by stirring at room temperature for 48 hours. Water was added to the reaction solution and the mixture was extracted with ethyl acetate. The organic layer was washed with water and dried over anhydrous magnesium sulfate, followed by concentration under reduced pressure. The residue was subjected to silica gel column chromatography (solvent; hexane : ethyl acetate = 3:1), and the resulting solid was further washed with a mixed solution of hexane-isopropyl ether (1:1) to give 325 mg of the title compound as a white powder (yield: 60%). Melting point 117-119C 1H-NMR spectrum (400 MHz, CDCl3) deltappm: 7.67 (1H, dd, J=9Hz, 5Hz), 7.16 (1H, dd, J=8Hz, 3Hz), 7.05-6.98 (2H, m), 6.83 (1H, s), 4.43-4.41 (1H, m), 4.26-4.01 (5H, m), 3.95-3.88 (1H, m), 2.56-2.45 (2H, m), 2.24-2.11 (1H, m), 1.88-1.80 (1H, m), 1.27 (3H, t, J=7Hz).

The synthetic route of 2106-02-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Daiichi Sankyo Company, Limited; EP1935879; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 13918-92-8, The chemical industry reduces the impact on the environment during synthesis 13918-92-8, name is 2,4-Difluorobenzene-1-sulfonyl chloride, I believe this compound will play a more active role in future production and life.

A mixture of 4.0 g (21.4 mmol) C-3, 4.3 mL (32.1 mmol) 2,4-difluorobenzenesulfonyl chloride, 5.2 mL (64.2 mmol) pyridine and 50 mL DCM is stirred at RT for 5 h. After completion of the reaction, the solvent is removed under reduced pressure, the crude product is taken up in 50 mL water and extracted twice with 100 mL DCM. The combined organic layers are dried over MgSO4 and the solvent is removed under reduced pressure. The crude product can be used without further purification. Yield: 7.88 g (91%).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 2,4-Difluorobenzene-1-sulfonyl chloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; WUNBERG, Tobias; KRAEMER, Oliver; van der VEEN, Lars; US2013/23533; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 626-43-7, 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 626-43-7 as follows.

General procedure: 14 Typical continuous diazotization procedure: Material A (50 mL of aqueous solution containing amine (100 mmol), fluoroboric acid (120 mmol), hydrochloric acid (180 mmol)), and material B (50 mL of aqueous solution containing sodium nitrite (105 mmol)) were pumped into the T-joint at 4 mL/min, respectively, after a residence time of about 15 s at 25 C in a reacting tube, the mixture flowed through the outlet and accumulated in the cooling vessel. Vigorous stirring was maintained. The solid was filtered with suction after the slurry was cooled to -5 C. The solid was washed with methanol and then dried in vacuo to yield the corresponding diazonium tetrafluoroborate. 15 Typical continuous fluorodediazoniation procedure: Slurry of the diazonium tetrafluoroborate prepared as above in 300 mL of cosolvent was introduced into a reacting tube continuously at a flow rate of 4 mL/min. The mixture was maintained for 1 min at setting temperature and then cooled in the tandem tube. The collected liquid was washed with aqueous NaOH and water, nearly colorless liquid was obtained.

According to the analysis of related databases, 626-43-7, the application of this compound in the production field has become more and more popular.

Reference:
Article; Yu, Zhi-Qun; Lv, Yan-Wen; Yu, Chuan-Ming; Su, Wei-Ke; Tetrahedron Letters; vol. 54; 10; (2013); p. 1261 – 1263;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

104-11-0, name is 1-(4-Chlorophenyl)-N-methylmethanamine, 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. name: 1-(4-Chlorophenyl)-N-methylmethanamine

REFERENTIAL EXAMPLE 2 Dissolved in toluene was 3.1 g (0.02 mole) of 4-chloro-N-methyl-benzylamine, followed by an addition of a catalytic amount of pyridine and a further dropwise addition of 1.8 g (0.022 mole) of diketene at room temperature. After stirring the reaction mixture at room temperature for 3 hours, it was poured in water and then extracted with toluene. Subsequent to purification, N-methyl-N-(4-chlorobenzyl)acetamide was obtained in an oily form.

The synthetic route of 104-11-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Kumiai Chemical Industry Co., Ltd.; Toyo Jozo Co., Ltd.; US4736038; (1988); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 4863-91-6, name is 3-Chloro-5-fluoroaniline, 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 4863-91-6, Application In Synthesis of 3-Chloro-5-fluoroaniline

EXAMPLE A-12 N-(3-chloro-5-fluorophenyl)-N’-t-pentylthiourea A solution of 8.5 g of 3-chloro-5-fluoroaniline in 150 ml of benzene was refluxed. To the solution was added 2.2 g of thiophosgene in 10 ml of benzene dropwise with stirring. The mixture was stirred at the same temperature for 3 hours, cooled to room temperature and filtered to remove insoluble matter. The filtrate was evaporated in vacuo and filtered again to remove insoluble matter. The filtrate was evaporated in vacuo. The residue was purified by silica gel column chromatography using n-hexane as a solvent. The resulting oil was dissolved in 30 ml of benzene and reacted with 3.4 g of t-pentylamine with stirring at room temperature for 30 minutes. The reaction mixture was evaporated in vacuo and the resulting solid recrystallized from cyclohexane to give 2.2 g of the title compound as colorless needles melting at 116.0-117.5 C. NMR (DMSO-d6, delta ppm): 0.82 (3H, t), 1.42 (6H, s), 1.93 (2H, q), 7.0-7.1 (1H, m), 7.4-7.7 (3H, m), 9.58 (1H, bs).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 3-Chloro-5-fluoroaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Kanebo, Ltd.; US5087640; (1992); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 15205-11-5,Some common heterocyclic compound, 15205-11-5, name is 2-Chloro-4-fluorobenzylamine, molecular formula is C7H7ClFN, 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 173; lambda/-[(2-chloro-4-fluorophenyl)methyl]-2-[1-(2-hydroxyethyl)-5- (trifluoromethyl)-1 H-pyrazol-4-yl]acetamide (E173) Crude [1-(2-hydroxyethyl)-5-(trifluoromethyl)-1 H-pyrazol-4-yl]acetic acid (6.0 g, -6.52 mmol, prepared as described below) was suspended in dimethylformamide (8 ml) and to this was added water soluble carbodiimide (1.5 g, 7.82 mmol), 1- hydroxybenzotriazole (1.06 g, 7.82 mmol), N-ethyl morpholine (2.49 ml, 19.56 mmol), and [(2-chloro-4-fluorophenyl)methyl]amine (1.25 g, 7.82 mmol). The mixture was stirred at room temperature overnight and then partitioned between ethyl acetate (50 ml) and water (50 ml). The organic phase was separated and washed with more water (2 x 20 ml), dried over anhydrous sodium sulphate, filtered, and concentrated to an orange oil. This material was purified by automated flash-silica column chromatography (Biotage SP4), eluting with 0-100% ethyl acetate in hexane, to give lambda/-[(2-chloro-4-fluorophenyl)methyl]-2-[1-(2-hydroxyethyl)-5-(trifluoromethyl)-1 H- pyrazol-4-yl]acetamide as a sticky white solid (~1 g). LC/MS [M+H]+ = 381 , retention time = 2.47 minutes.

The synthetic route of 15205-11-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXO GROUP LIMITED; WO2008/138876; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 328-72-3, 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. 328-72-3, name is 3,5-Bis(trifluoromethyl)chlorobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 10 Synthesis of 3,5-bis(trifluoromethyl)cinnamide (Method II) 0.181 g (2.55 mmol) of acrylamide, 9.7 mg (30 mumol) of NBu4Br, 0.675 mg (3 mumol) of palladium acetate and 2.67 mg (12 mumol) of phenyldi(t-butyl)phosphine are weighed into a Schlenk vessel. 0.542 g (3 mmol) of 3,5-bis(trifluoromethyl)chlorobenzene and 0.637 ml (3 mmol) of dicyclohexylmethylamine and also 2.5 ml of dimethylacetamide are then added. The Schlenk vessel is placed in a heating bath at 130 C. and the contents are stirred. After 3 hours, the yield is determined by means of HPLC: 99% (TON=723, TOF=241/h).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 3,5-Bis(trifluoromethyl)chlorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Rampf, Florian; Eckert, Markus; US2003/105353; (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. 56961-77-4, name is 1-Bromo-2,3-dichlorobenzene, A new synthetic method of this compound is introduced below., Application In Synthesis of 1-Bromo-2,3-dichlorobenzene

Intermediate 40:[0172] A well-dried flask was first charged with l-bromo-2,3-dichlorobenzene (10 g, 44 mmol) and piperazine (4.55 g, 53 mmol), which was evacuated and backfilled with N2 through a balloon under gentle warming (40C). Toluene was charged and the mixture was bubbled with N2 for 10 min, then BINAP (822 mg, 1.32 mmol) and Pd2dba3 (403 mg, 0.44 mmol) were added to the mixture. After the addition of DBU (8.0 mL), the solution was warmed at 60-70C while a fine powder of ffluONa (7.39 g, 66 mmol) was added in one portion to start the amination. After the reaction mixture cooled to rt, (Boc)20 (24 g, 110 mmol) was dissolved in DCM and added dropwise to the reaction mixture, then stirred at rt for 3 h. The reaction mixture was diluted with water and extracted with EtOAc. The combined EtOAc layers were washed with brine, dried over anhydrous Na2S04, concentrated in vacuo and purified by flash chromatography on silica gel column (elution with PE/EtOAc = 10:1) to give tert-butyl 4-(2,3-dichlorophenyl)piperazine-l- carboxylate (intermediate 40) (11.1 g, 76%) as a white solid.

The synthetic route of 56961-77-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; THE UNIVERSITY OF NORTH CAROLINA AT CHAPEL HILL; JIN, Jian; ROTH, Bryan; FRYE, Stephen; WO2012/3418; (2012); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

32768-54-0, name is 2,3-Dichlorotoluene, 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. Formula: C7H6Cl2

Example 1: Synthesis of 2,3-dichlorobenzotrichloride; A UV photochlorination reactor was loaded with 245 g of 2,3-dichlorotoluene (1.52 moles) and 1225 g of CCl4. The reactor was heated to 75 0C and chlorine was introduced at a flow of 190 g/h. At the end of the reaction, the flow is decreased to minimize break-through of chlorine. The crude mixture was analyzed showing a content of 2,3-dichlorobenzal chloride < 0.2 %. The solvent CCl4 was distilled from the reaction mixture at 600 to 800 mbar. The crude product was then let to distil at 13 mbar and 128 0C giving 334.2 g of 2,3- dichlorobenzotrichloride with a GC assay of 98.2 %. Yield was 81.6 %.; Example 3: Synthesis of 2,3-dichlorobenzotrichloride; A UV photochlorination reactor was loaded with 220.5 g of 2,3-dichlorotoluene (1.37 moles) and 1584 g of CCl4. The reactor was heated to 75 0C and chlorine was introduced at a flow of 190 g/h. At the end of the reaction, the flow was decreased to minimize break-through of chlorine. The crude mixture was analyzed showing a content of 2,3-dichlorobenzal chloride < 0.2 %. The solvent was distilled from the reaction mixture (1808 g) giving 1351 g of CCl4. The crude 2,3-dichlorobenzotrichloride (366.5 g) had a GC assay of 96.0 %. Yield was 97.1%.; Example 5: Synthesis of 2,3-dichlorobenzotrichloride; A UV photochlorination reactor was loaded with 1042 g of 2,3-dichlorotoluene (6.47 moles). The reactor was heated to 100 0C and chlorine was introduced at a flow of 370 g/h. At the end of the reaction, the flow was decreased to 40 g/h to minimize break-through of chlorine. The crude mixture was analysed showing a content of 2,3-dichlorobenzal chloride of 0.3 %. The 2,3-dichlorobenzotrichloride (1675.5 g) was obtained with a GC assay of 97.2 %. Yield was 95.2 %. The synthetic route of 32768-54-0 has been constantly updated, and we look forward to future research findings. Reference:
Patent; CALAIRE CHIMIE SAS; WO2007/138075; (2007); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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 14490-19-8 as follows. category: chlorides-buliding-blocks

A pressure vessel was charged with l,4-dichloropyrido[4,3-d]pyridazine (prepared according to the procedures in WO2009/035568A1) (66 mg, 0.33 mmol, 1.0 eq.), 3-trifluoromethyl aniline (0.05 mL, 0.39 mmol, 1.2 eq.) and l-methyl-2-pyrrolidinone (0.1 mL). The reaction was sealed and was heated to 105 C for 1 h. Analysis showed mono- addition as the major product with a minor amount of bis-addition product. Regioisomeric mono-addition products were not observed. The reaction was then cooled to room temperature and was diluted with water and saturated sodium bicarbonate solution. The mixture was extracted with ethyl acetate (2X). The combined organic layer was dried with sodium sulfate, was filtered and was concentrated to give the crude product. The product was purified by column chromatography (eluted with hexanes:ethyl acetate = 4: 1 to 1 : 1) to afford l-chloro-N-(3- (trifluoromethyl)phenyl)pyrido[4,3-d]pyridazin-4-amine (41 mg, 38% yield). MS (EI) for C14H8CIF3 4: 325 (MH+), Chlorine isotope pattern.

According to the analysis of related databases, 14490-19-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; EXELIXIS, INC.; ANAND, Neel, Kumar; BROWN, S., David; TESFAI, Zerom; ZAHARIA, Cristiana, A.; WO2012/37132; (2012); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics