反应详情

Butyllithium (143 ml of 1.4 molar solution in hexane) was added dropwise to a stirred solution of caprolactam (11.3 g) in dry tetrahydrofuran under nitrogen. After stirring for 50 minutes at 0°, 3-methoxy-2-cyclohexenone (12.6 g) in tetrahydrofuran was added. After a further 30 minutes the reaction was poured onto 5 M hydrochloric acid. The organic layer was separated and the aqueous layer was extracted with chloroform. The combined organic layers were dried over magnesium sulphate. Removal of the solvent under reduced pressure left 15 g of a yellow solid. The product was recrystallised from ethyl acetate affording 2.5 g of the title compound identical to that described in Example 17.

1. customThe organic layer was separated
2. extractionthe aqueous layer was extracted with chloroform
3. dry with materialThe combined organic layers were dried over magnesium sulphate
4. customRemoval of the solvent under reduced pressure
5. waitleft 15 g of a yellow solid
6. customThe product was recrystallised from ethyl acetate affording 2.5 g of the title compound identical to