反应详情

An ice-chilled solution of sodium hydroxide (1.9 g) in water (25 ml) was added, during 40 minutes, to a stirred solution of 4-methyl-3-oxo-pentanoic acid ethyl ester (3 g, 18.96 mmoles) and 1,2-dichloro-1-ethoxy-ethane (3.3 g, 35.19 mmole) in diethyl ether (15 ml) with ice bath cooling. When the addition was complete the mixture was stirred rapidly for 1 hour, then the ethereal layer was separated, washed with water and dried. Evaporation of the solvent gave a yellow oil, which was purified by flash chromatography using a gradient elution from neat pentane to pentane/diethyl ether 9:1 v/v as eluent, to afford compound 82 as an oil (2.4 g).

1. temperaturecooling
2. additionWhen the addition
3. customthe ethereal layer was separated
4. washwashed with water
5. customdried
6. customEvaporation of the solvent
7. customgave a yellow oil, which
8. customwas purified by flash chromatography
9. washa gradient elution from neat pentane to pentane/diethyl ether 9:1 v/v as eluent