反应详情

Reflux a suspension of 5.0 g. of dl-13-ethyl-3-methoxygona-1,3,5(10)-trien-17β-ol and 3.83 g. of sodium hydride (50% in oil) for 1.5 hours in xylene (100 ml). Add 14.5 ml. of ethyl iodide and reflux for 22 hours. Acidify with 2N hydrochloric acid and extract the material with benzene. Chromatograph the residue on alumina (Grade I neutral). Elute the product with benzene-ether (1:1). Recrystallize the product from 60 ml. of methanol to obtain dl-17β-ethoxy-13-ethyl-3-methoxygona-1,3,5(10)-triene (2.3 g); m.p. 74°-77°C.

1. temperatureReflux
2. additiona suspension of 5.0 g
3. additionAdd 14.5 ml
4. extractionAcidify with 2N hydrochloric acid and extract the material with benzene
5. washElute the product with benzene-ether (1:1)
6. customRecrystallize the product from 60 ml