HRID1296275

反应详情

EQUATION

反应方程式

HRID 1296275 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirring solution of N,N-diethyl-4-hydroxy-2-(trifluormethoxy)benzamide (1876 mg, 6.8 mmol) and diisopropylethylamine (1747 mg, 13.5 mmol) in dry DMF (60 mL) was added chloro(1,1-dimethylethyl)dimethylsilane (1123 mg, 7.5 mmol). The reaction was stirred for 16 h and then quenched with 1M HCl. The reaction was extracted with EtOAc (3×50 mL). The organic layers were combined, dried over Na2SO4, and conc. in vacuo to a pale yellow oil. The oil was purified by flash chromatography (silica gel, 0–40% EtOAc in hexanes) to give 1941 mg of the desired product as a colorless oil. MS (ESI) 392 (M+H).

WORKUP

后处理

  1. customquenched with 1M HCl
  2. extractionThe reaction was extracted with EtOAc (3×50 mL)
  3. dry with materialdried over Na2SO4
  4. customThe oil was purified by flash chromatography (silica gel, 0–40% EtOAc in hexanes)