Adding a certain compound to certain chemical reactions, such as: 461432-23-5, name is 4-Bromo-1-chloro-2-(4-ethoxybenzyl)benzene, 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 461432-23-5, category: chlorides-buliding-blocks
To the mixture of 10 cc THF and 10 cc Toluene added 0.138 mole 4-(5-bromo-2- chlorobenzyl)phenyl ethyl ether at ambient temperature and stirred for 15 min. Cooled to -70 to -80C in dry ice /acetone bath and stirred for 15 min. Added a solution of 0.014 mole n-Butyl lithium (1.9M in hexanes) at -70 to -80C. and stirred for lhr. Added solution of 3, 4, 5-Tris-trimethylsilanyloxy-6-trimethylsilanyloxymethyl-tetrahydro- pyran-2-one in 5 cc of Toluene at -70 to -80C and stirred for 2 to 3hrs. After the compliance of the reaction, reaction mass was quenched with Methane sulphonic acid and Allyl alcohol mixture at -70 to -80C. Temperature was raised to ambient temperature and stirred overnight. Reaction mass was quenched with 30 cc sat.sodiumbicarbonate solution to bring the pH neutral to alkaline and stirred for 30.0 min. Layers separated and aqueous layer was extracted with 10 cc of Toluene. Organic layer was combined and washed with 30cc water and 50 cc sat. brine solution. Organic layer was distilled under reduced pressure to recover toluene. Solid compound was dissolved in 50cc of toluene and quenched in n-Hexane to obtain 83 % the compound as crystalline solid. HPLC purity: 88 – 91 % I R data: Anomeric C-0 stretching: 1242 cm”1 Allylic C- O stretching: 1 177 cm”1 Allylic C- H stretching: 3010 – 3120 cm”1 Aromatic C- CI stretching: 820 cm”1 Lactones O – H stretching: 3240 – 3380 cm”1 Lactones C – 0 stretching: 1045 – 1092 cm”1 Aromatic C=C stretching: 1510 , 1548 , 1603 , 1703 cm”1 Alkane C – H stretching: 2877,2866, 2956, 2958, 2962 cm”1 Aromatic C – H stretching: 3050 – 3090 cm”1 Dip-Mass (M+Na) 487.19 m/z (M+K) 503.17 m/z
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Bromo-1-chloro-2-(4-ethoxybenzyl)benzene, and friends who are interested can also refer to it.
Reference:
Patent; HARMAN FINOCHEM LIMITED; KADAM, Vijay Trimbak; SAIKRISHNA; CHOUDHARE, Tukaram Sarjerao; MINHAS, Harpreet Singh; MINHAS, Gurpreet Singh; (26 pag.)WO2016/147197; (2016); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics