HRID267542

反应详情

EQUATION

反应方程式

HRID 267542 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To 500 ml isopropanol was added 30 g. (1.0 mole) of paraformaldehyde and 137 g. (1.0 mole) of 2-amino-1-phenylethanol, and the resulting mixture was stirred and heated at 50°C. After the solids had all dissolved, the solution was stirred an additional 30 minutes at 50°C. To the solution, cooled to 35°C., was added 68.7 g. (0.375 mole) of anhydrous zinc acetate and 76.0 g. (1.0 mole) of carbon disulfide. Solids formed in several minutes whereby additional isopropanol (400 ml) was added to stir the mixture efficiently. After heating at 55°C. for two hours, the mixture was cooled and filtered; the resulting solids were washed several times in a Waring Blendor with water, and air-dried overnight to obtain 184 g (95%) of the desired product melting at 220°-223°C.; its IR spectrum was consistent with the structure.

WORKUP

后处理

  1. temperatureTo the solution, cooled to 35°C.
  2. additionwas added 68.7 g
  3. additionwas added
  4. stirringto stir the mixture efficiently
  5. temperatureAfter heating at 55°C. for two hours
  6. temperaturethe mixture was cooled
  7. filtrationfiltered
  8. washthe resulting solids were washed several times in a Waring Blendor with water
  9. customair-dried overnight