HRID2266868

反应详情

EQUATION

反应方程式

HRID 2266868 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To sodium cyanide (18.4 g, 375 mmol) and ammonium carbonate (39.0 g, 500 mmol) in H2O (450 mL) was added 2-methyl-4,4,4-trifluorobutanal (17.5 g, 125 mmol) in ethanol (450 mL). The reaction mixture was heated to 90° C. for 17 h. After cooling to 25° C., about 500 mL of solvent was removed in vacuo. Concentrated HCl was added to acidify the mixture to a pH of about 1 to about 2 and a precipitate formed. The mixture was filtered and washed with aqueous 1 N HCl to give 5-(3,3,3-trifluoro-1-methylpropyl)imidazolidine-2,4-dione as a white solid (15.5 g, 59%).

WORKUP

后处理

  1. temperatureAfter cooling to 25° C.
  2. customabout 500 mL of solvent was removed in vacuo
  3. additionConcentrated HCl was added
  4. customa precipitate formed
  5. filtrationThe mixture was filtered
  6. washwashed with aqueous 1 N HCl