反应详情

A solution of 41 g. of 3-hydroxy-3-methyl-2-butanone in 300 ml. of dry tetrahydrofuran was treated at -10° under nitrogen with 500 ml. of 2M benzyl magnesium chloride and stirred at 25° C. for 20 hours. An aqueous ammonium chloride solution was added at 0° and the mixture was acidified at 0° with concentrated hydrochloric acid and extracted with ethyl acetate. The extract was evaporated and the residue chromatographed on silica gel. Elution with 20% ethyl acetate in hexane followed by recrystallization from the same solvent afforded 38 g. of the title product, m.p. 72°-74°, λmaxKBr 2.95, 3.35, 6.2, 6.63, 6.82, 7.23, 7.45, 7.65, 8.32, 8.70, 9.13, 10.58, 11.0, 11.40, 12.30, 12.97 and 14.06 μ.

1. extractionextracted with ethyl acetate
2. customThe extract was evaporated
3. customthe residue chromatographed on silica gel
4. washElution with 20% ethyl acetate in hexane
5. customfollowed by recrystallization from the same solvent
6. customafforded 38 g