HRID1578120

反应详情

EQUATION

反应方程式

HRID 1578120 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.81 g (0.02 mol) of benzoyl chloride were added in drops in 20 minutes and at a temperature of 0°-5° C. to a solution of N-(2',2'-dimethoxy-ethyl)-2,6-dimethyl aniline (4.45 g; 0.02 mol) in ethyl ether (20 ml) containing triethylamine (2.76 ml; 0.02 mol). The reaction mixture was stirred at room temperature for 15 minutes. The resulting salt was filtered and the solution was washed with 8 ml of an aqueous solution of hydrochloric acid at 5% and then with water up to neutral pH. The organic phase was anhydrified with anhydrous NaSO4 and the solvent was evaporated, so obtaining 5.2 g of a white solid which, recrystallized from petroleum ether (25 ml) provided 4.5 g of product (purity=91% by GLC) with a yield of 65.5% (white solid, melting point=58°-59° C.).

WORKUP

后处理

  1. filtrationThe resulting salt was filtered
  2. washthe solution was washed with 8 ml of an aqueous solution of hydrochloric acid at 5%
  3. customthe solvent was evaporated