反应详情

温度

40 °C

A mixture of 900 mg of the product from Step B, 1 ml of methyl carbonate and 15 ml of dimethylformamide was heated to 40° C. and 360 mg of sodium hydride in a 50% oil suspension were added thereto portion wise and the mixture was stirred for 6 hours at room temperature. The mixture was poured into an aqueous hydrochloric acid solution and was extracted with petroleum ether (b.p.= 40°-75° C.). The extracts were washed with water, dried over sodium sulfate and evaporated to dryness. The residue was chromatographed over silica and was eluted with a 7-3 petroleum ether-ethyl ether mixture to obtain 374 mg of methyl 11-methoxy-7,11-dimethyl-3-oxo-6-dodecenoate in the form of a colorless oil.

1. extractionwas extracted with petroleum ether (b.p.= 40°-75° C.)
2. washThe extracts were washed with water
3. dry with materialdried over sodium sulfate
4. customevaporated to dryness
5. customThe residue was chromatographed over silica
6. washwas eluted with a 7-3 petroleum ether-ethyl ether mixture