HRID1448920

反应详情

EQUATION

反应方程式

HRID 1448920 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

19.6 g (0.35 mole) of freshly distilled acrolein is added dropwise at a maximum of 50° C., with ice-cooling, to a solution of 27.8 g (0.2 mole) of N-(3-pent-2-enyl)-pyrrolidine in 50 ml of benzene. After completion of the addition, the mixture is stirred overnight at room temperature; it is subsequently heated for 2 hours at 50°-55° C. and then concentrated by evaporation. The oil remaining is dissolved in 250 ml of 20% hydrochloric acid and the solution is stirred overnight. Extraction is then performed five times with ether; the combined extracts are dried over magnesium sulphate and the ether is distilled off. The crude 2,6-dimethyl-cyclohex-2-en-1-one remaining is purified by vacuum distillation. There is obtained 14.8 g (60% of theory) of 2,6-dimethyl-cyclohex-2-en-1-one, b.p. 62°-64° C./ 10 Torr.

WORKUP

后处理

  1. additionAfter completion of the addition
  2. temperatureit is subsequently heated for 2 hours at 50°-55° C.
  3. concentrationconcentrated by evaporation
  4. dissolutionThe oil remaining is dissolved in 250 ml of 20% hydrochloric acid
  5. stirringthe solution is stirred overnight
  6. extractionExtraction
  7. dry with materialthe combined extracts are dried over magnesium sulphate
  8. distillationthe ether is distilled off
  9. distillationThe crude 2,6-dimethyl-cyclohex-2-en-1-one remaining is purified by vacuum distillation