HRID1658597

反应详情

EQUATION

反应方程式

HRID 1658597 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-phenethyl-5-chloro-2-methoxybenzamide (10 g.) dissolved in 25 ml. of chloroform was cooled to -10° and 19 g. of chlorosulfonic acid was added dropwise, maintaining the temperature at -10° to 0°. After the addition was complete the mixture was allowed to rise to room temperature and it was poured onto cracked ice. The crude sulfonic acid was filtered and 7.3 g. (57%) was obtained. A sample recrystallized for analysis from alcohol-acetonitrile melted at 188°-189°. Anal. Calcd. for C16H16ClNO5S: C, 51.94; H, 4.36; Cl, 9.58; N, 3.79; S, 8.67. Found: C, 50.10; H, 4.27; Cl, 9.93; N, 4.04; S, 8.84.

WORKUP

后处理

  1. temperaturemaintaining the temperature at -10° to 0°
  2. additionAfter the addition
  3. customto rise to room temperature
  4. additionit was poured
  5. filtrationThe crude sulfonic acid was filtered
  6. custom(57%) was obtained
  7. customA sample recrystallized for analysis from alcohol-acetonitrile melted at 188°-189°