反应详情

24.3 g of 1-bromo-6,6-dimethylhept-2-en-4-yne in 750 ml of ethanol are added at -50° to 245 ml of a 33% ethanolic solution of methylamine and the mixture stirred in a closed vessel at 55° for 3 hours. The resulting mixture is concentrated in a rotary evaporator and the residue taken up with chloroform and washed with 1 N NaOH and saturated NaCl. After drying over MgSO4 the crude product is purified by chromatography on kieselgel (eluant toluene/ethylacetate; 4/1). A colourless oil is obtained (trans- and cis compound in ratio 3:1).

1. concentrationThe resulting mixture is concentrated in a rotary evaporator
2. washwashed with 1 N NaOH and saturated NaCl
3. dry with materialAfter drying over MgSO4 the crude product
4. customis purified by chromatography on kieselgel (eluant toluene/ethylacetate; 4/1)
5. customA colourless oil is obtained (trans- and cis compound in ratio 3:1)