HRID1858086

反应详情

EQUATION

反应方程式

HRID 1858086 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 5-allyl-4-chloro-2-[2-(3,5-dimethylphenyl)-acetylamino]-benzoic acid methyl ester (1.4 g in 40 mL dry tetrahydrofuran) at 0° C. was added dropwise a solution of sodium bis(trimethylsilyl)amide (9.8 mL of a 1.0M solution in tetrahydrofuran) and the mixture warmed to room temperature. After 4 hours, the reaction was cooled to 0° C. and quenched by the addition of of 200 mL iced 6N hydrochloric acid. The slurry was stirred for 15 minutes then filtered and washed sequentially with ice water (500 mL), cold hexane (200 mL) and cold toluene (100 mL). The residue was dried in vacuo to give the title compound (960 mg).

WORKUP

后处理

  1. temperaturethe reaction was cooled to 0° C.
  2. customquenched by the addition of of 200 mL iced 6N hydrochloric acid
  3. filtrationthen filtered
  4. washwashed sequentially with ice water (500 mL), cold hexane (200 mL) and cold toluene (100 mL)
  5. customThe residue was dried in vacuo