反应详情

1.4 g of 4-acetyl-1-methyl-1-cyclohexanecarboxylic acid (Example 36) was dissolved in 50 ml of DMF, and 5 g of potassium carbonate and 3 ml of allyl bromide were added to the resultant solution. The solution was reacted for 6 hours at room temperature. After reaction, 100 ml of an aqueous sodium chloride solution was added to the reaction solution. The solution was extracted three times with 30 ml of methylene chloride. The organic layer obtained was washed three times with an aqueous sodium chloride solution and dried over magnesium sulfate. Thereafter, the solvent was removed in vacuo. The oily substance obtained was subjected to column chromatography using 20 g of silica gel. From the fraction eluted with hexane and ethyl acetate=10:1, the solvent was removed in vacuo, yielding obtaining 1.5 g of allyl 4-acetyl-1-methyl-1-cyclohexanecarboxylate as a colorless oil, which had the following physiochemical properties:

1. customThe solution was reacted for 6 hours at room temperature
2. additionwas added to the reaction solution
3. extractionThe solution was extracted three times with 30 ml of methylene chloride
4. customThe organic layer obtained
5. washwas washed three times with an aqueous sodium chloride solution
6. dry with materialdried over magnesium sulfate
7. customThereafter, the solvent was removed in vacuo
8. customThe oily substance obtained
9. washFrom the fraction eluted with hexane and ethyl acetate=10:1
10. customthe solvent was removed in vacuo
11. customyielding