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 (900 mg) was dissolved in THF (10 mL), water (2 mL), and Et3N (1.8 mL) prior to the addition of 1M i-propyl chloroformate (4.5 mL) in toluene. The reaction was stirred for 4 h 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 CH2Cl2 to give the title compound (800 mg). MS found: (2M−1)−=581.2.

1. concentrationthe solution was concentrated to a white solid
2. dissolutionA portion of this material (900 mg) was dissolved in THF (10 mL)
3. additionwater (2 mL), and Et3N (1.8 mL) prior to the addition of 1M i-propyl chloroformate (4.5 mL) in toluene
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 CH2Cl2