反应详情

温度

50 °C

A mixture of 13.4 g (0.12 mol) of potassium tert-butoxide and 100 g of tert-butanol was stirred and heated until the tert-butoxide totally dissolved. The solution was cooled to about 50° C. and 17 g (0.12 mmol) of ethyl 2-methylacetoacetate was added dropwise. Ethyl-6-bromohexanoate (30 g, 0.13 mmol) was then added dropwise and the reaction mixture was stirred and refluxed for 5 hours. The mixture was filtered and the solvent was removed under reduced pressure. The residue was partitioned between 1M HCl and chloroform. The organic layer was dried over magnesium sulfate and purified on silica gel using 1:10 ethyl acetate/hexane as the eluent to yield 25 g (75%) of diethyl 2-acetyl-2-methyloctanedioate (3) as yellow liquid.

1. dissolutiontotally dissolved
2. stirringthe reaction mixture was stirred
3. temperaturerefluxed for 5 hours
4. filtrationThe mixture was filtered
5. customthe solvent was removed under reduced pressure
6. customThe residue was partitioned between 1M HCl and chloroform
7. dry with materialThe organic layer was dried over magnesium sulfate
8. custompurified on silica gel using 1:10 ethyl acetate/hexane as the eluent