反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Trifluoroacetic acid (2 mL) was added to a solution of 1,1-dimethylethyl 3-[({3-{[(1S)-1-methyl-2-(methyloxy)ethyl]oxy}-5-[(3-methyl-4-oxo-3,4-dihydro-2H-1,3-benzoxazin-7-yl)oxy]phenyl}carbonyl)amino]-1H-pyrazole-1-carboxylate (190 mg, 0.34 mmol) in DCM (12 mL) and stirred at RT for 2 hours. The solvent was removed in vacuo and DCM (20 mL) added and the mixture washed with water (20 mL), saturated sodium bicarbonate solution (20 mL), brine (20 mL), dried (MgSO4), and reduced in vacuo to give the desired compound as a white solid (54 mg). 1H NMR δ (CDCl3): 1.32 (d, 3H), 3.09 (s, 3H), 3.40 (s, 3H), 3.47-3.63 (m, 2H), 4.56-4.63 (m, 1H), 5.16 (s, 2H), 6.52 (d, 1H), 6.71-6.74 (m, 1H), 6.81 (t, 1H), 6.85 (s, 1H), 7.18 (s, 1H), 7.37 (s, 1H), 7.49 (s, 1H), 7.92 (d, 1H), 9.46 (s, 1H), 9.46 (s, 1H); m/z 453 (M+H)+
WORKUP
后处理
- customThe solvent was removed in vacuo and DCM (20 mL)
- additionadded
- washthe mixture washed with water (20 mL), saturated sodium bicarbonate solution (20 mL), brine (20 mL)
- dry with materialdried (MgSO4)