HRID1857627

反应详情

EQUATION

反应方程式

HRID 1857627 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]-benzoic acid methyl ester (3.05 g in 20 mL dry tetrahydrofuran) at 0° C. was added dropwise a solution of sodium bis(trimethylsilyl)amide (20 mL of a 1.0M solution in tetrahydrofuran) and the mixture warmed to room temperature. After 2 hours, the reaction was cooled to 0° C. and quenched by the addition of 100 mL iced 6N hydrochloric acid. The slurry was stirred for 15 minutes then filtered and washed (2×) with ice cold acetonitrile. The residue was dried in vacuo overnight to give the title compound (2.3 g).

WORKUP

后处理

  1. temperaturethe reaction was cooled to 0° C.
  2. customquenched by the addition of 100 mL iced 6N hydrochloric acid
  3. filtrationthen filtered
  4. washwashed (2×) with ice cold acetonitrile
  5. customThe residue was dried in vacuo overnight