反应详情

A solution of 3-hydroxy-5-methoxy-4-nitrophenylacetic acid (0.76 g, Reference Example 12) in methanol (100 mL) and concentrated hydrochloric acid (5 drops) was heated at reflux through 3A molecular sieve for 4 hours, then evaporated. The residue was partitioned between ethyl acetate and water. The organic phase was washed with water, then with brine, then dried and then evaporated. The residue was subjected to flash chromatography on silica eluting with dichloromethane, then with a mixture of methanol and dichloromethane (1:49, v/v) to give the title compound (0.34 g).

1. customevaporated
2. customThe residue was partitioned between ethyl acetate and water
3. washThe organic phase was washed with water
4. dry with materialwith brine, then dried
5. customevaporated
6. additionwith a mixture of methanol and dichloromethane (1:49, v/v)