HRID1157630

反应详情

EQUATION

反应方程式

HRID 1157630 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2,2,2-trifluoro-N-{2-methyl-5-[(trimethylsilyl)ethynyl]phenyl}-acetamide (10.9 g, 36 mmol) in THF (350 mL) cooled to 0° C. was added a 1M solution of tetrabutylammonium fluoride in THF (40 mmol, 40 mL). The reaction was diluted with water and extracted two times with EtOAc. The combined organic extractions were washed with water, dried over MgSO4 and concentrated onto silica gel. The crude material was purified by column chromatography to give the desired product (6.4 g, 78%). 1H NMR (400 MHz, d6-DMSO) δ 11.00 (s, 1H), 7.36-7.30 (m, 3H), 4.19 (s, 1H), 2.17 (s, 3H) ppm.

WORKUP

后处理

  1. extractionextracted two times with EtOAc
  2. extractionThe combined organic extractions
  3. washwere washed with water
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated onto silica gel
  6. customThe crude material was purified by column chromatography