HRID1018549

反应详情

EQUATION

反应方程式

HRID 1018549 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

Sodium hydride (34 mg, 60%) was suspended in N-methyl-2-pyrrolidone (2 mL) and 8-(3,5-bis-trifluoromethyl-benzoyl)-1-phenyl-1,3,8-triaza-spiro[4.5]decan-4-one (200 mg) was added with stirring. After 5 minutes stirring at room temperature 4-(2-chloroethyl)morpholine hydrochloride (79 mg) was added. The mixture was heated to 100° C. with stirring and kept for 1 h at that temperature. After cooling, saturated sodium bicarbonate solution was added and the mixture was extracted with ethylacetate. Organic phases were pooled, dried with Na2SO4 and the solvent was evaporated. Chromatography on silica gel (ethylacetate) yielded the desired product (180 mg, 73%), MS: m/e=585.1 (M+H+).

WORKUP

后处理

  1. additionwas added
  2. stirringwith stirring
  3. temperatureAfter cooling
  4. extractionthe mixture was extracted with ethylacetate
  5. dry with materialdried with Na2SO4
  6. customthe solvent was evaporated