HRID1047572

反应详情

EQUATION

反应方程式

HRID 1047572 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-Methyl-4-(2-(5-nitro-1-(tetrahydro-2H-pyran-2-yl)-1H-indazol-3-yl)-1H-benzo[d]imida-zol-5-yl)morpholine (60 mg, 0.130 mmol) was added to 10% Pd/C (10 mg) in ethanol (25 mL) and then hydrogen gas (60 psi) was applied for 8 h at room temperature. The reaction mixture was filtered through Celite, and the solvent was removed in vacuo. Purification by flash chromatography (5% CH3OH/CH2Cl2) afforded the title compound (40 mg). 1H NMR: (400 MHz, CD3OD): δ 7.66 (d, 1H, J=2.0 Hz), 7.52 (m, 2H), 7.13 (s, 1H), 7.04-7.00 (m, 2H), 5.79 (dd, 1H, J=2.4 and 9.2 Hz), 3.97 (m, 2H), 3.79 (m, 3H), 3.49 (m, 1H), 3.41 (m, 1H), 2.76 (m, 1H), 2.62 (m, 1H), 2.44 (m, 1H), 2.13 (m, 1H), 2.05 (m, 1H), 1.80 (m, 1H), 1.68 (m, 2H), 1.22 (d, 3H, J=6.4 Hz); ESI-MS [M+H]+: 433.2.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered through Celite
  2. customthe solvent was removed in vacuo
  3. customPurification by flash chromatography (5% CH3OH/CH2Cl2)