HRID1875772

反应详情

EQUATION

反应方程式

HRID 1875772 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

To a solution of 2-(4-cyano-2-fluoro-phenoxymethyl)-benzoic acid methyl ester (2.17 g, 7.6 mmol) in tetrahydrofuran (30 ml) was added a solution of lithium hydroxide monohydrate (1.59 g, 38.03 mmol) in water (30 ml) and the resulting mixture was allowed to stir at 25° C. for 12 h. The solvent was removed in vacuo, the residue was diluted with water (20 ml), washed with diethyl ether (2×15 ml). The aqueous layer was then acidified to pH 5 with 2N aqueous hydrochloric acid and extracted with ethyl acetate (2×40 ml). The combined organic layers were washed with water (2×25 ml), brine, dried over sodium sulfate, filtered, and evaporated to afford the desired compound as a colorless solid (90%). MS (Turbo Spray): m/z=272.1 (M+H).

WORKUP

后处理

  1. customThe solvent was removed in vacuo
  2. additionthe residue was diluted with water (20 ml)
  3. washwashed with diethyl ether (2×15 ml)
  4. extractionextracted with ethyl acetate (2×40 ml)
  5. washThe combined organic layers were washed with water (2×25 ml), brine
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. customevaporated