HRID1418489

反应详情

EQUATION

反应方程式

HRID 1418489 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

Methanethiol was bubbled into a stirred suspension of sodium hydride (65% w/w dispersion in mineral oil, 273 mg, 7.4 mmol) in DMF (10 ml) until a clear solution was obtained. 4-Cyano-4-(3,5-difluorophenyl)-3,4,5,6-tetrahydro-2H-pyran (1.65 g, 7.4 mmol) was added and the resulting mixture was heated at 100° C. for 22 h, cooled and poured into water (100 ml). The mixture was extracted with Et2O (100 ml) and extract washed with water (100 ml), brine (100 ml) and dried (MgSO4). Removal of solvent gave 1.87 g (quant.) of the titled compound as a tan oil.

WORKUP

后处理

  1. customwas obtained
  2. temperaturecooled
  3. extractionThe mixture was extracted with Et2O (100 ml)
  4. extractionextract
  5. washwashed with water (100 ml), brine (100 ml)
  6. dry with materialdried (MgSO4)
  7. customRemoval of solvent