HRID349378

反应详情

EQUATION

反应方程式

HRID 349378 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-amino-3-methylbenzoic acid (6 g) in dry 1,4-dioxane (50 mL) was added dropwise a solution of trichloromethyl chloroformate (8 mL) in dry 1,4-dioxane (25 mL), with ice-water cooling to keep the reaction temperature below 25° C. A white precipitate began to form during the addition. The reaction mixture was stirred at room temperature overnight. The precipitated solids were removed by filtration and washed with 1,4-dioxane (2×20 mL) and hexane (2×15 mL) and air-dried to yield 6.51 g of off-white solid.

WORKUP

后处理

  1. customthe reaction temperature below 25° C
  2. customto form during the addition
  3. customThe precipitated solids were removed by filtration
  4. washwashed with 1,4-dioxane (2×20 mL) and hexane (2×15 mL)
  5. customair-dried