HRID1475338

反应详情

EQUATION

反应方程式

HRID 1475338 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 1-[6-(3-chloro-propane-1-sulfonyl)-5-fluoro-3,3-dimethyl-2,3-dihydro-indol-1-yl]-ethanone (502 mg, 1.44 mmol) at −78° C. in THF (30 mL) under N2, KHMDS (0.5 M in toluene, 3 mL) was slowly added. The solution was stirred for 10 minutes at the same temperature and then 30 minutes at ambient temperature then quenched with 1 M hydrochloric acid and extracted with EtOAc. The organic phase was dried (MgSO4), filtered and concentrated. The crude material was purified by SiO2 chromatography (EtOAc:Petrol 1:1) to give the title compound (310 mg). MS: [M+H]+=312.

WORKUP

后处理

  1. custom30 minutes at ambient temperature then quenched with 1 M hydrochloric acid
  2. extractionextracted with EtOAc
  3. dry with materialThe organic phase was dried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe crude material was purified by SiO2 chromatography (EtOAc:Petrol 1:1)