反应详情

2-(tert-Butoxycarbonyl)amino-5-trifluoromethylbenzoic acid (6.0 g) was dissolved in 4M HCl (4 mL) in dioxane. After 3 h, the solution was concentrated to a white solid. A portion of this material (200 mg) was dissolved in THF (2.5 mL) and 2M K2CO3 (1.46 mL) was added followed by cyclohexanecarbonyl chloride (0.2 mL). The reaction was stirred for 10 min before EtOAc was added. The EtOAc layer was washed with 1N HCl and brine before it was dried, filtered, and concentrated to a crude material. This material was crystallized with CH3CN to give the title compound (302 mg). MS found: (2M−1)−=629.2.

1. concentrationthe solution was concentrated to a white solid
2. dissolutionA portion of this material (200 mg) was dissolved in THF (2.5 mL)
3. addition2M K2CO3 (1.46 mL) was added
4. additionwas added
5. washThe EtOAc layer was washed with 1N HCl and brine before it
6. customwas dried
7. filtrationfiltered
8. concentrationconcentrated to a crude material
9. customThis material was crystallized with CH3CN