HRID2375918

反应详情

EQUATION

反应方程式

HRID 2375918 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Pd/C (17 mg, 10%, with 50% water) was added into the suspension of 1-methyl-6-nitro-1H-1,3-benzimidazole (85.0 mg, 0.480 mmol) in ethanol (3 mL). The mixture was degassed and filled with H2. The mixture was stirred at rt under balloon pressure for 16 h. After that time, the mixture was filtered and concentrated in vacuo to obtain the title compound as pink crystals. 1H NMR (CD3OD, 400 MHz): δ=3.67 (s, 3H), 6.69-6.73 (m, 2H), 7.33 (dd, 1H, J=0.4 & 8.8 Hz), 7.77 (s, 1H). MS (ES+): m/z 148.16 (100) [MH+]. HPLC: tR=0.43 min (ZQ2000, polar—5 min).

WORKUP

后处理

  1. customThe mixture was degassed
  2. additionfilled with H2
  3. filtrationAfter that time, the mixture was filtered
  4. concentrationconcentrated in vacuo