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 10061-02-6 as follows. 10061-02-6

To a 3000 mL three-necked flask equipped with a thermometer, a condenser, a constant pressure dropping funnel and a stirrer, 437.2 g (1.0 mol) of fipronil, 60 g (1.5 mol) of NaOH and 1500 mL of ethanol were added, 138.8 g (1.25 mol) of 1,3-trans-dichloropropene was added dropwise at -10 C, and after completion of the dropwise addition, the temperature was controlled at -10 C for 24 hours. The reaction was completed, filtered, the filtrate was adjusted with concentrated hydrochloric acid system pH to neutral, under 40 C vacuum solvent recovery, the residue was slowly added dropwise to ice water, the temperature was controlled at 0 ~ 5 crystallization, filtration, residue by methanol Crystallization, filtration, drying, to give a white crystalline solid 390.0g. Yield 72.8%, liquid chromatography quantitative analysis of content of 95.5%.

According to the analysis of related databases, 10061-02-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Hunan Chemical Institute Co., Ltd.; Du Shenghua; Lan Shilin; Liu Weidong; Liu Yuan; Huang Chaoqun; Wang Yanli; Luo Liangming; (6 pag.)CN105949126; (2016); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

13526-66-4, These common heterocyclic compound, 13526-66-4, name is 3-Bromo-6-chloroimidazo[1,2-b]pyridazine, 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.

To a mixture of 3-bromo-6-chloro-1-yl-imidazo[1,2-b]pyridazine (1.00 g, 4.3 mmol) in 1,2-dimethoxy ethane (1 mL) was added diisopropyl ethyl amine (0.5 mL) and 1-BOC-piperazine (2.41 g, 13 mmol). The mixture was degassed (4 cycles of vacuum and nitrogen) and heated at 120 C. for 27 hours. The reaction mixture was cooled to room temperature, treated with saturated aqueous sodium bicarbonate (100 mL) and extracted with ethyl acetate (2¡Á100 mL). The organic layers were combined and dried with magnesium sulfate, filtered and evaporated to a residue, which was purified by chromatography on silica gel; elution with a gradient of hexane/ethyl acetate gave 4-(3-bromo-imidazo[1,2-b]pyridazine-6-yl)-piperazine-1-carboxylic acid tert-butyl ester as an off-white solid (1.01 g, 83%): mp 176-9 C.; LC/MS [M+H]+ 382, 384.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 13526-66-4.

Reference:
Patent; ALCON MANUFACTURING, LTD.; US2008/153813; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

1435-48-9, 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. 1435-48-9, name is 2,4-Dichloro-1-fluorobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Add NaH (60% in mineral oil, 0.132 g, 3.32 mmol) to 1- (benzyl-methyl-amino)-4-methyl-3-ol (0.498 g, 2.21 mmol) in anhydrous DMSO (10 mL). After 30 minutes, add 1, 3-dichloro-4- fluorobenzene (0.474 g, 2.87 mmol) and then heat the reaction mixture at 60C overnight. Cool the mixture and partition between EtOAc and water. Separate the layers and extract the aqueous layer with EtOAc. Combine the organic extracts, wash with aqueous saturated sodium chloride solution, dry over anhydrous Na2SO4, filter, and concentrate in vacuo. Purify the residue on silica gel eluting with 5% 2N NH3 in MeOH/dichloromethane to give benzyl- [3- (2, 4-dichloro- phenoxy) -4-methyl-pentyl] -methyl amine (0.385 g, 48%). Mass spectrum (ion spray): m/z = 366 (M+1),’H NMR (CD30D) 8 734 (d, 1H), 7.28-7. 17 (m, 6H), 7.06 (d, 1H), 4.35-4. 31 (m, 1H), 3.48 (dd, 2H), 2.55-2. 43 (m, 2H), 2.19 (s, 3H), 1.98-1. 83 (m, 3H), 0.98 (dd, 6H).

The synthetic route of 1435-48-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ELI LILLY AND COMPANY; WO2005/92835; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

50638-47-6, These common heterocyclic compound, 50638-47-6, name is 4-Bromo-2-chloro-1-methoxybenzene, 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.

To a magnetically stirring solution of 4-bromo-2-chloroanisole (0.50 g, 2.61 mmol) and 1-Cyclopentyl-2-propen-1-ol (1.5 eq, 0.49 g, 3.88 mmol) in anhydrous N-methylpyrrolidinone (3.0 mL), under argon at room temperature, was added sodium bicarbonate (1.2 eq, 0.26 g, 3.10 mmol) followed by dichlorobis (triphenylphosphine) palladium (II) (0.02 eq, 36.7 mg, 0.05 mmol). The resulting mixture was heated to 140 C. in an oil bath and maintained for 4 hours. The resulting dark reaction mixture was cooled to room temperature and poured into water (50 mL) and extracted with EtOAc (2¡Á25 mL). The organics were washed with water (50 mL) and brine (50 mL) then dried over Na2SO4, filtered and concentrated. The crude residue was purified by flash chromatography (1% through 10% EtOAc in Hexanes) to yield the intermediate ketone as a slightly yellow oil (0.49 g, 79%).

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 50638-47-6.

Reference:
Patent; Agouron Pharmaceuticals, Inc.; US2005/176701; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

1435-48-9, A common heterocyclic compound, 1435-48-9, name is 2,4-Dichloro-1-fluorobenzene, molecular formula is C6H3Cl2F, 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.

To a solution of 2,4-Dichloro-1-fluorobenzene (165.0 g, 1.0 mol) in THF (500 mL) n-BuLi (420 mL, 2.5 M, 1.05 mol) was added at -78 C. After stirring at -78 C for 1 h, Oxirane (44.0 g, 1.0 mmol) was added and stirred at -78 C for 2 h. The mixture was quenched with sat. NH4Cl solution, extracted with EtOAc (200 mL * 3). The organic phase was washed with water (100 mL * 2), brine (100 mL * 2), dried over Na2SO4. After filtering, the organic phase was concentrated to give compound 44 as a colorless liquid (156.7 g, 75.0% yield). 1H NMR (400 MHz, CDCl3) delta 7.29-7.25 (m, 1H, Ar-H), 7.02-6.97 (m, 1H, Ar-H), 3.89-3.84 (m, 2H, CH2), 3.29-3.24 (m, 2H, CH2).

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

Reference:
Article; Liu, Na; Wang, Yanfen; Huang, Gongchao; Ji, Conghui; Fan, Wei; Li, Haitao; Cheng, Ying; Tian, Hongqi; Bioorganic Chemistry; vol. 65; (2016); p. 146 – 158;,
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. 3972-56-3, name is 1-tert-Butyl-4-chlorobenzene, This compound has unique chemical properties. The synthetic route is as follows., 3972-56-3

General procedure: An oven-dried Schlenk tube was evacuated and backfilled with nitrogen. The Schlenk tube was charged with Pd(bda)2 (11.5 mg,0.02 mmol), L1 (13.7 mg, 0.03 mmol), K3PO4 (424.5 mg, 2 mmol), and toluene (1.0 mL). After stirring for 15 min, the solution of arylhalide (1.0 mmol) and phenol (1.2 mmol) in toluene (1.5 mL) was added. The septum was replaced with an inside reflux condenser, and then the reaction mixture was stirred for 18 h at 110 C. Then,the reaction mixture was cooled to room temperature and quenched with water (5 mL). After separating the organic phase, the aqueous phase was extracted with ethyl acetate (3 mL3), and the combined organic phase was dried over anhydrous Na2SO4. The solvent was concentrated under reduced pressure, and then the crude material was purified by column chromatography on silica gel

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; Zhang, Yi; Ni, Gang; Li, Chengjun; Xu, Sheng; Zhang, Zhaoguo; Xie, Xiaomin; Tetrahedron; vol. 71; 30; (2015); p. 4927 – 4932;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

106131-61-7, The chemical industry reduces the impact on the environment during synthesis 106131-61-7, name is 3,6-Dichloro-1,2,4,5-tetrazine, I believe this compound will play a more active role in future production and life.

General procedure: Dichloro-s-tetrazine (1 mmol) and fluorinated alcohol (1 mmol) were dissolved in anhydrous dichloromethane (10 mL). 2,4,6-collidine (1 mmol) was added dropwise at room temperature in the solution, and the mixture was stirred for 12 h under N2 atmosphere.The solvent was evaporated and the residue was passed through a column of silica (2/8 dichloromethane/petroleum ether v/v) to give compound 2 as a pink solid, with a ?yellow? fluorescence on TLC (using a standard laboratory UV lamp with a broad band centred at 365 nm).

The chemical industry reduces the impact on the environment during synthesis 3,6-Dichloro-1,2,4,5-tetrazine. I believe this compound will play a more active role in future production and life.

Reference:
Article; Ben Chaabane, Radhia; Guermazi, Refka; Clavier, Gilles; Audebert, Pierre; Hedhli, Ahmed; Dyes and Pigments; vol. 108; (2014); p. 64 – 69;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

6276-54-6, 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. 6276-54-6 name is 3-Chloropropan-1-amine hydrochloride, 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.

di-tert-butyl dicarbonate(10.89 g, 50mmol)was dissolved in 50 ml THF. The solutionwas cooledto 0 C. 3-Chloropropan-1-amine hydrochloride (6.46 g, 69 mmol) wasdissolved in 20 ml of 1 M NaOH solution and added using a droppingfunnel, and the solution was stirred overnight. 150 ml of ethyl acetatewere added and extraction was performed. The organic phase waswashed three times with water and once with brine, and then driedover magnesium sulfate. The solvent was removed and a viscous oilwas produced, which was dried under vacuum (7.27 g, 68%). 1H NMR(400 MHz, CDCl3) delta (ppm): 4.80 (bs, NH), 3.53 (t, J = 6.4 Hz, 2H),3.22 (q, J = 6.4 Hz, 2H), 1.91 (quin, J = 6.4 Hz, 2H),1.42 (s, 9 H). 13CNMR (100 MHz, CDCl3, delta, ppm): 156, 79, 42, 37, 32, 28.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Chloropropan-1-amine hydrochloride, and friends who are interested can also refer to it.

Reference:
Article; Weiss, Ester; Gertopski, Diana; Gupta, Maneesh Kumar; Abu-Reziq, Raed; Reactive and functional polymers; vol. 96; (2015); p. 32 – 38;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

72934-36-2, 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. 72934-36-2 name is 1-(4-Chlorophenyl)cyclopropanamine, 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.

To a slurry of tert-butyl 4-(4-chloro-6-(2,2,2-trifluoroethoxy)-1,3,5-triazin-2-ylamino)benzoate (3.6 g) and 1-(4-chlorophenyl)cyclopropanamine (1.49 g) in THF (50 mL) was stirred for 5 hours at 80 C. The precipitate was filtrated through a plug washing with THF to give a crude product that was purified by Biotage eluting with 4/1-hexane/ethyl acetate to give 1.8 g of tert-butyl 4-(4-(1-(4-chlorophenyl)cyclopropylamino)-6-(2,2,2-trifluoroethoxy)-1,3,5-triazin-2-ylamino)benzoate as a solid.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-(4-Chlorophenyl)cyclopropanamine, and friends who are interested can also refer to it.

Reference:
Patent; WANG, TAO; Yin, Zhiwei; Scola, Paul Michael; US2014/135335; (2014); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

73006-78-7, The chemical industry reduces the impact on the environment during synthesis 73006-78-7, name is 5-Chloro-[1,1′-biphenyl]-2-amine, I believe this compound will play a more active role in future production and life.

A mixture of the product from step (i) (0.94g), sodium acetate (0.5g) and tert- butylbromoacetate (0.6ml) in ethanol (20ml) was heated under reflux for 5h. A further porton of sodium acetate (Ig) and tert-butylbromoacetate( 1.2ml) was added and the mixture heated under reflux overnight. The solvent was evaporated under reduced pressure and the residue partitioned between ethyl acetate and water, the organic layer was washed with water, dried, and the solvent evaporated under reduced pressure. The residue was purified by chromatography on silica eluting with 5% ethyl acetate/isohexane, yield 0.775g. MS: APCI (-ve) 260 (M-l-tBu)

The chemical industry reduces the impact on the environment during synthesis 5-Chloro-[1,1′-biphenyl]-2-amine. I believe this compound will play a more active role in future production and life.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2006/37982; (2006); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics