HRID1856381

反应详情

EQUATION

反应方程式

HRID 1856381 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 18.2 g (0.20 m) of thiosemicarbazide in 250 ml of hot water was gradually added to a solution of 26.4 g (0.20 m) of cinnamaldehyde in 250 ml of hot 2B ethanol. Small, colorless crystals began to ppt from the homogeneous mixture after several minutes of heating on a steam bath. Heating was continued for a half an hour, after which the mixture was cooled to room temperature and the product was collected by filtration, washed with cold ethanol, and air-dried to yield 25.5 g of small, pale yellow crystals. An additional 18.3 g of product was recovered by concentrating the mother liquors. Recrystallization from ethanol gave 29.3 g (0.14 m) of small, pale yellow crystals, m.p. 137°-139° C.

WORKUP

后处理

  1. waitto ppt from the homogeneous mixture after several minutes
  2. temperatureof heating on a steam bath
  3. temperatureHeating
  4. waitwas continued for a half an hour
  5. filtrationthe product was collected by filtration
  6. washwashed with cold ethanol
  7. customair-dried
  8. customto yield 25.5 g of small, pale yellow crystals
  9. customAn additional 18.3 g of product was recovered
  10. concentrationby concentrating the mother liquors
  11. customRecrystallization from ethanol
  12. customgave 29.3 g (0.14 m) of small, pale yellow crystals, m.p. 137°-139° C.