反应详情

A mixture of potassium tert-butoxide (68 g) and tert-butanol (130 ml) was treated dropwise with a mixture of 3-methylbenzaldehyde (33.8 g) and methyl crotonate (45 ml). The temperature of the reaction mixture rose to 65° C. during the addition and this was maintained for a further 3 hours. The reaction mixture was cooled to room temperature, poured into ice/water and washed with diethyl ether. The aqueous phase was acidified with concentrated HCl and extracted with diethyl ether. The organic phase was washed with water, dried (MgSO4) and evaporated under reduced pressure. Purification was by trituration with isohexane and filtration.

1. additionThe temperature of the reaction mixture rose to 65° C. during the addition
2. temperaturethis was maintained for a further 3 hours
3. washwashed with diethyl ether
4. extractionextracted with diethyl ether
5. washThe organic phase was washed with water
6. dry with materialdried (MgSO4)
7. customevaporated under reduced pressure
8. customPurification
9. filtrationwas by trituration with isohexane and filtration