反应详情

To a solution of 4-(biphenyl-4-ylmethoxycarbonylamino)-biphenyl-3-carboxylic acid methyl ester (0.51 g, 1.179 mmol) in THF (5 mL) was added at room temperature 1.0 M LiOH (2.42 mL, 2.42 mmol) and the mixture was stirred for 3 h. The solvent was evaporated, water was added, followed by 2N HCl to adjust the pH to 1-2, and the product was extracted with ethyl acetate. The extract was washed with water, then brine, and dried over magnesium sulfate, concentrated to dryness and purified by chromatography to yield 0.317 g of 4-(biphenyl-4-ylmethoxycarbonylamino)-biphenyl-3-carboxylic acid 601, mp: 234.5-235.6° C.

1. customThe solvent was evaporated
2. additionwater was added
3. extractionthe product was extracted with ethyl acetate
4. washThe extract was washed with water
5. dry with materialbrine, and dried over magnesium sulfate
6. concentrationconcentrated to dryness
7. custompurified by chromatography