反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionAfter completion of the addition
- temperatureit is subsequently heated for 2 hours at 50°-55° C.
- concentrationconcentrated by evaporation
- dissolutionThe oil remaining is dissolved in 250 ml of 20% hydrochloric acid
- stirringthe solution is stirred overnight
- extractionExtraction
- dry with materialthe combined extracts are dried over magnesium sulphate
- distillationthe ether is distilled off
- distillationThe crude 2,6-dimethyl-cyclohex-2-en-1-one remaining is purified by vacuum distillation