Category: 98577-44-7

Related Products of 98577-44-7, A common heterocyclic compound, 98577-44-7, name is 1,1-Dibromo-2,2-bis(chloromethyl)cyclopropane, molecular formula is C5H6Br2Cl2, 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.

Step 1 : A flame-dried pressure tube was charged with l,l-dibromo-2,2- bis(chloromethyl)cyclopropane (15 g, 50.5 mmol) and dibutyl ether (15 mL). The reaction was cooled to -45 C and PhLi (53.2 mL, 101 mmol, 1.8M in dibutyl ether) was added slowly via syringe. The mixture was stirred at the same temperature for 5 mins. The reaction temperature was allowed to warm to 0 C and stirred for 2 h in an ice bath at which point the reaction was brought to RT to provide a solution of crude [l. l. l]propellane.

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; KALYRA PHARMACEUTICALS, INC.; BUNKER, Kevin, Duane; HUANG, Peter, Qinhua; ABRAHAM, Sunny; PINCHMAN, Joseph, Robert; HOPKINS, Chad, Daniel; SLEE, Deborah, Helen; (93 pag.)WO2017/205459; (2017); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 98577-44-7, name is 1,1-Dibromo-2,2-bis(chloromethyl)cyclopropane, 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 98577-44-7, Quality Control of 1,1-Dibromo-2,2-bis(chloromethyl)cyclopropane

(1) Equipment specifications: three-stage 1000mL CSTR reactor (continuous stirring tank reactor, full mixed anaerobic reactor), 50ml plunger pump, 5000g balance, 1.0L feeding bottle. (2) Proportion of raw materials: Solution A: 5.0 kg of 1,1-dibromo-2,2-chloromethylcyclopropane + 2.0 vol n-butyl ether, L1 (feed rate of solution A) = 4.5 g / min; Solution B: 2.2eq lithium phenyl / n-butyl ether solution, L2 (feed rate of solution B) = 4.5g / min; Solution C: 1.0 g / g ammonia; L3 (feed rate of solution C) = 1.0 g / min. (3) Reaction conditions: three-stage CSTR, the first-stage low-temperature section is controlled at -50 to 0 C, and the retention volume is 500ml; the second and third-stage reaction sections are controlled at 0 C, the retention volume is 700ml, and the third-stage overflow To the receiving bottle, the temperature of the receiving bottle was controlled at 0 C, the total retention volume was 1200 ml, and the RT (retention time) = 2.0 h. Turn on the automatic feeding system, two feeds, L1 = 4.5g / min, L2 = 4.5g / min, the two feeds are mixed through the low-temperature section of the first-stage CSTR, and after 40 minutes, overflow to the second- and third-stage reaction sections After 70 minutes of reaction, the third-stage CSTR began to overflow to the receiving bottle, and the charging system was started. L3 = 1.0 g / min, and the reaction was quenched by continuous injection of ammonia water. Post-treatment, liquid separation, and low-temperature distillation gave 0.761 kg (converted content) of the product, and the NMR yield was 68%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,1-Dibromo-2,2-bis(chloromethyl)cyclopropane, and friends who are interested can also refer to it.

Reference:
Patent; Jilinkai Laiying Pharmaceutical And Chemical Co., Ltd.; Hong Hao; Zhang Enxuan; Lu Jiangping; Wei Fuliang; Yang Sihang; (11 pag.)CN110117215; (2019); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

A common heterocyclic compound, 98577-44-7, name is 1,1-Dibromo-2,2-bis(chloromethyl)cyclopropane, molecular formula is C5H6Br2Cl2, 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. 98577-44-7.

Tricyclo [1.1.1.01’3] pentane Methyllithium (46.3 mL, 74.1 mmol, 1.6M in diethyl ether) was added to a solution of l,l-dibromo-2,2-bis(chloromethyl)cyclopropane (10 g, 33.7 mmol) in pentane (10 mL) stirred at -78C for 15 min. After the reaction mixture was maintained at -78C for 15 min, the reaction flask was removed from the dry ice/acetone bath and placed in an ice-water bath. The reaction mixture was stirred at that temperature for 2 hrs. The volatiles, which was warmed at 40C by using an oil bath, were collected via a shortpath distillation condenser under a dry-ice-acetone environment. The condensed material was used in next reaction without further purification.

The synthetic route of 1,1-Dibromo-2,2-bis(chloromethyl)cyclopropane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; YEUNG, Kap-Sun; EASTMAN, Kyle J.; PARCELLA, Kyle E.; WO2014/159559; (2014); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics