HRID548731

反应详情

EQUATION

反应方程式

HRID 548731 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe solvent was removed in vacuo and DCM (20 mL)
  2. additionadded
  3. washthe mixture washed with water (20 mL), saturated sodium bicarbonate solution (20 mL), brine (20 mL)
  4. dry with materialdried (MgSO4)