反应详情

A mixture of 5E (3.80 g) and tetrahydrofuran (12 ml) was heated to reflux in 2N sodium hydroxide (12 ml) for 12 hours. Then the mixture was poured on ice and acidified with 6N sulfuric acid (pH=1-2). The mixture is extracted with diethyl ether twice. The combined organic phases were washed with water and dried. The mixture was concentrated and the residue is distilled under reduced pressure to yield the product as a white solid (3.22 g, 89%) with a melting point of 142-144° C.

1. temperaturewas heated
2. additionThen the mixture was poured on ice
3. extractionThe mixture is extracted with diethyl ether twice
4. washThe combined organic phases were washed with water
5. customdried
6. concentrationThe mixture was concentrated
7. distillationthe residue is distilled under reduced pressure