反应详情

To a solution of 3-{3-[(3,5-bis-trifluoromethyl-benzoyl)-methyl-amino]-pyridin-4-yl}-4-methyl-benzoic acid methyl ester (33 mg, 66.5 μmol, example 83) in dioxane (1 mL) was added water (2 mL) and LiOH.H2O (3.49 mg, 83.1 μmol). The reaction mixture was stirred at room temperature for 2 hours and then poured on 20 mL 1M aqueous HCl and 20 mL EtOAc. The layers were separated and the aqueous layer extracted a second time with 20 mL EtOAc. The combined organic layers were washed with 20 ml brine, dried over MgSO4, filtered and concentrated under vacuum. Colorless solid (32 mg, 99%). MS (ESI): m/z=483.113 [M+H]+.

1. customThe layers were separated
2. extractionthe aqueous layer extracted a second time with 20 mL EtOAc
3. washThe combined organic layers were washed with 20 ml brine
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated under vacuum