HRID2098131

反应详情

EQUATION

反应方程式

HRID 2098131 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirring mixture of the above crude 6-(trifluoromethyl)quinolin-2(1H)-one in DMF/THF (0.5 M, 1:1) at rt was added NaH portionwise (1.2 g, 30.88 mmol) over 15 min. The reaction mixture was stirred at rt for additional 20 min before a solution of bromo methyl acetate (4.73 g, 30.88 mmol) in THF was added. The resulting mixture was stirred at rt until the starting material was consumed. The mixture was slowly quenched with brine and extracted with EtOAc. The crude product mixture was purified by column chromatography (3.6 g, 82% in two steps). Retention time (min)=2.042, method [1], MS (ESI) 286.1 (M+H).

WORKUP

后处理

  1. additionwas added
  2. customwas consumed
  3. customThe mixture was slowly quenched with brine
  4. extractionextracted with EtOAc
  5. customThe crude product mixture was purified by column chromatography (3.6 g, 82% in two steps)