反应详情

A mixture of 7 grams of 5,6,7,8-tetrahydro-1-methyl4(1H)-cycloheptapyrazolone, 2.3 grams of sodium hydride (97%), 12 ml of ethyl formate, 2 drops of ethanol and 100 ml of tetrahydrofuran was heated at reflux for 3 hours. The mixture was then cooled and partitioned between water and ether. The aqueous layer was washed once with ether and acidified to a pH of 5 with 1 N hydrochloric acid. The white precipitate which formed was separated by filtration and dried to give 5,6,7,8-tetrahydro-5-hydroxymethylene-1-methyl-4(1H)-cycloheptapyrazolone as a cream colored powder melting at about 133°-135° C.

1. temperaturewas heated
2. temperatureat reflux for 3 hours
3. temperatureThe mixture was then cooled
4. custompartitioned between water and ether
5. washThe aqueous layer was washed once with ether
6. customThe white precipitate which formed
7. customwas separated by filtration
8. customdried