2-bromo-1-chloro-4-(chloromethyl)benzene synthesis

Yield:880348-46-9 88%

Reaction Conditions:

with tetrachloromethane;triphenylphosphine in dichloromethane; for 18 h;

Steps:

1.A

A. 3-Bromo-4-chlorobenzyl chloride.; To a solution of 3-bromo-4-chlorobenzyl alcohol (9.6 g, 43 mmol) in CH₂Cl₂ (100 mL) was added Ph₃P (17.1 g, 1.5 mmol) and CCl₄ (6.3 mL, 65 mmol). After 18 h, the solution was washed with brine (3×100 mL) and passed through a short silica gel column to afford the product as,colorless oil (9.14 g, 88%). ¹H NMR (400 MHz, CDCl₃): 7.65 (d, J=2.1 Hz, 1H), 7.43 (d, J=8.2 Hz, 1H), 7.27 (dd, J=8.3, 2.1 Hz, 1H), 4.51 (s, 3H).

References:

US2006/69286,2006,A1 Location in patent:Page/Page column 72