反应详情

温度

0 °C

n-Butyllithium (14.4 ml, 2.5M solution in hexane) was added dropwise to a stirred solution of the product from step (i) (6.9 g) in THF (100 ml) at 0° C. The solution was stirred at 0° C. for 1 hour and then transferred by cannula into a solution of 4-chloromethyl-1-methoxy-2-methylbenzene (J. Chem. Soc. 1956, 2455) (5.86 g) in THF (60 ml) at -30° C. The mixture was stirred for 1 hour and allowed to warm to room temperature. After 30 minutes the reaction was quenched with water. The mixture was partitioned between ethyl acetate and water. The organic phase was washed with water, dried (MgSO4) and evaporated. Purification was by chromatography eluting with 5% ethyl acetate in isohexane. Yield 2.16 g.

1. stirringThe mixture was stirred for 1 hour
2. temperatureto warm to room temperature
3. customAfter 30 minutes the reaction was quenched with water
4. customThe mixture was partitioned between ethyl acetate and water
5. washThe organic phase was washed with water
6. dry with materialdried (MgSO4)
7. customevaporated
8. customPurification
9. washeluting with 5% ethyl acetate in isohexane