HRID1858090

反应详情

EQUATION

反应方程式

HRID 1858090 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 4-chloro-2-[2-(3,5-dimethylphenyl)-acetylamino]-5-iodo-benzoic acid methyl ester (EXAMPLE 4.1B, 10.9 g in 180 mL dry tetrahydrofuran) at 0° C. was added dropwise 59.5 mL of a 1 M solution of sodium bis(trimethylsilyl)amide in tetrahydrofuran and the mixture allowed to warm to room temperature. After 1.5 hours, the mixture was cooled to 0° C. and the reaction quenched by the addition of 400 mL ice:6N hydrochloric acid (1:1). This was stirred for 15 minutes then filtered to collect the solid product. The solids were washed with ice-water then cold acetonitrile and dried to give the title compound (9.8 g).

WORKUP

后处理

  1. temperaturethe mixture was cooled to 0° C.
  2. customthe reaction quenched by the addition of 400 mL ice
  3. filtrationthen filtered
  4. customto collect the solid product
  5. washThe solids were washed with ice-water
  6. dry with materialcold acetonitrile and dried