反应详情

2-Amino-4-(trifluoromethyl)benzoic acid (714 mg, 3.48 mmol), propionylaldehyde (0.27 ml, 3.74 mmol), acetic acid (3.49 mmol) and sodium triacetoxyborohydride (1.12 g, 5.25 mmol) were added in THF (40 ml). The reaction mixture was stirred overnight. The reaction mixture was quenched by adding sat. NaHCO3 (50 ml). The aqueous mixture was extracted with CH2Cl2 (30 ml×3). A combined organic layer was dried over MgSO4, concentrated in vacuo, and purified with column chromatography to yield title compound (155 mg, 18%).

1. customThe reaction mixture was quenched
2. additionby adding sat. NaHCO3 (50 ml)
3. extractionThe aqueous mixture was extracted with CH2Cl2 (30 ml×3)
4. dry with materialA combined organic layer was dried over MgSO4
5. concentrationconcentrated in vacuo
6. custompurified with column chromatography