HRID1380519

反应详情

EQUATION

反应方程式

HRID 1380519 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-10 °C

PROCEDURE

实验过程

A mixture of 21.0 g of 1,1-diphenylacetone and 40 ml of N,N-dimethylformamide dimethyl acetal in a 300 ml round bottom flask was heated in an oil bath at 120° C. for 8 hours with ethanol being distilled over. The reaction mixture was cooled and evaporated in vacuo to give an oil. The oil was boiled up in 50 ml of ether then cooled at -10° C. and gave a heavy precipitate. The precipitate was collected, washed with ether, then air dried and gave 21.5 g of crude product. A 5.0 g portion was recrystallized from 50 ml of 2-propanol, then cooled at room temperature. The material was collected and dried at 60° C. and gave 1.7 g of the desired product, mp 93°-94° C.

WORKUP

后处理

  1. distillationdistilled over
  2. temperatureThe reaction mixture was cooled
  3. customevaporated in vacuo
  4. customto give an oil
  5. customgave a heavy precipitate
  6. customThe precipitate was collected
  7. washwashed with ether
  8. customair dried
  9. customgave 21.5 g of crude product
  10. customA 5.0 g portion was recrystallized from 50 ml of 2-propanol
  11. temperaturecooled at room temperature
  12. customThe material was collected
  13. customdried at 60° C.