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