HRID1511897

反应详情

EQUATION

反应方程式

HRID 1511897 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

5-(4-octylphenyl)dihydrofuran-3(2H)-one (0.8 g, 2.92 mmol) and ammonium carbonate (1.037 g, 13.12 mmol) (Aldrich) were combined in ethanol (12.05 ml) and water (12.05 ml). Potassium cyanide (0.209 g, 3.21 mmol) (Fluka) was added and the reaction heated at about 80° C. for about 16 h. Cool the reaction and add concentrated HCl until acidic (caution for HCN gas formation). The precipitate was collected by vacuum filtration and washed with water. It was suspended in methylene chloride, filtered, and washed with methylene chloride to provide 8-(4-octylphenyl)-7-oxa-1,3-diazaspiro[4.4]nonane-2,4-dione (0.545 g, 1.582 mmol, 54.3% yield) as a white solid:

WORKUP

后处理

  1. temperatureCool
  2. customthe reaction
  3. filtrationThe precipitate was collected by vacuum filtration
  4. washwashed with water
  5. filtrationfiltered
  6. washwashed with methylene chloride