HRID1054492

反应详情

EQUATION

反应方程式

HRID 1054492 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of Na2CO3 (11.7 g, 110.7 mmol) in water (50 mL) and 1,4-dioxane (50 mL) at 60° C. was added 2-amino-4-chloro-benzoic acid (5.0 g, 29.14 mmol) followed by 4-chloro-3-trifluoromethyl-benzenesulfonyl chloride (20.15 g, 72.48 mmol) in 3 portions and heated the resulting reaction mixture at 80° C. for 4 hours. 2N HCl Was added until the reaction mixture became acidic (pH=˜2) and obtained white solid was filtered, washed with water, dried under high vacuum to obtain title compound (7.8 g) in 65% yield. MS (ES) M+Na expected 436.0. found 435.8.

WORKUP

后处理

  1. temperatureheated
  2. customthe resulting reaction mixture at 80° C. for 4 hours
  3. customobtained white solid
  4. filtrationwas filtered
  5. washwashed with water
  6. customdried under high vacuum