反应详情

A solution of 0.53 mL (10 mmol) of MeCN in 5 ml of THF was cooled in −78° C. bath and 12 mL of 1M LiN(TMS)2 was added. After 5 min, 0.75 mL (5.2 mmol) of methyl cyclohexane carboxylate was added. The cold bath was removed after 1 hr and stirring was continued for another 1 hr. The reaction was acidified with 1.2 N HCl and extracted with ether. The ether layer was washed with brine, dried and concentrated. The residue was chromatographed using a gradient of 10-50% EtOAc-hexane to furnish the desired product.

1. customThe cold bath was removed after 1 hr
2. waitwas continued for another 1 hr
3. extractionextracted with ether
4. washThe ether layer was washed with brine
5. customdried
6. concentrationconcentrated
7. customThe residue was chromatographed