反应详情

A solution of diethylamine (548 ml, 5.3 moles) in CH2Cl2 (452 ml) was added dropwise to a solution of 3-benzyloxy-4-methoxy-benzoyl chloride (146.66 g, 0.53 moles), obtained as described in example 30, in methylene chloride (640 ml), at 0° C. under nitrogen, at constant temperature. At the end the temperature was left to arise to the room value. After 2 hours the mixture was evaporated, taken up with ethyl acetate and washed with water. The organic phase was dried and concentrated to give a solid which, triturated twice with heptane and once with petrolatum, then dried at 45° C. under vacuum gave 150.62 g of the title compound (yield: 91%).

1. customobtained
2. waitAt the end the temperature was left
3. customAfter 2 hours the mixture was evaporated
4. washwashed with water
5. customThe organic phase was dried
6. concentrationconcentrated
7. customto give a solid which
8. customtriturated twice with heptane and once with petrolatum
9. customdried at 45° C. under vacuum