反应详情

To a solution of 5,5-bis(2-fluoro-4-methylphenyl)-4-(1-methyl-1H-tetrazol-5-yl)-2,4-pentadienal (1.3 g, 3.4 mmoles) in tetrahydrofuran (15 mL) at -50 ° C. was added the dianion of t-butyl acetoacetate (3.4 mL of a 1M solution, 3.4 mmoles). After stirring for 2 hours, another 0.7 mL of dianion solution was added and the solution stirred for an additional hour. The reaction was quenched with 1N hydrochloric acid and the mixture extracted with methylene chloride. The extracts were dried (MgSO4) and concentrated. The residue was purified by column chromatography on silica gel eluting with 1% (v/v) methanol in methylene chloride to give 1.3 g of the title compound; m.p.=55°-63° C.

1. additionanother 0.7 mL of dianion solution was added
2. stirringthe solution stirred for an additional hour
3. customThe reaction was quenched with 1N hydrochloric acid
4. extractionthe mixture extracted with methylene chloride
5. dry with materialThe extracts were dried (MgSO4)
6. concentrationconcentrated
7. customThe residue was purified by column chromatography on silica gel eluting with 1% (v/v) methanol in methylene chloride