反应详情

温度

0 °C

To a solution of the ketone from Step C (22 g) in dry tetrahydrofuran (400 ml) at 0° C. under nitrogen was added a solution of methyl lithium in diethyl ether (100 ml of 1.4M). The solution was stirred for 1 hr at 0° C. then water was cautiously added and solvents evaporated to give an aqueous mixture which was extracted with ether (2×150 ml). The combined extracts were washed with water, dried and evaporated. Crystallisation from ether/hexane gave 3,5-dimethyl-5H-dibenzo[a,d]cyclohepten-5-ol (20.18 g), m.p. 102°-103° C.

1. customsolvents evaporated
2. customto give an aqueous mixture which
3. extractionwas extracted with ether (2×150 ml)
4. washThe combined extracts were washed with water
5. customdried
6. customevaporated
7. customCrystallisation from ether/hexane