反应详情

To a solution of 2-methyl-3-buten-2-ol (4.1 g, 0.048 mole) in dry ether (10 ml) stirred under dry nitrogen at 5° C. was added a solution of n-butyllithium (19.3 ml, 0.048 mole, 2.5M in hexane). After completion of the addition, ethyl 2-(2-butyl)malonyl chloride (10.0 g, 0.048 mole) was added slowly with stirring, and an additional 10 ml quantity of ether was added. The suspension was stirred for 2 hours with warming to room temperature. The resultant suspension was extracted with water, a saturated ammonium chloride solution, and then water again. The layers were separated and the organic layer dried over magnesium sulphate, filtered, and subjected to reduced pressure distillation. The pale yellow liquid obtained was subjected to fractional distillation. A heart cut of 8.0 g (64.5%), b.p. 69°-71° C. at 0.1 mm, was obtained.

1. additionwas added slowly
2. stirringThe suspension was stirred for 2 hours
3. extractionThe resultant suspension was extracted with water
4. customThe layers were separated
5. dry with materialthe organic layer dried over magnesium sulphate
6. filtrationfiltered
7. distillationsubjected to reduced pressure distillation
8. customThe pale yellow liquid obtained
9. distillationwas subjected to fractional distillation
10. customA heart cut of 8.0 g (64.5%), b.p. 69°-71° C. at 0.1 mm, was obtained