HRID2375918
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
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
- customThe mixture was degassed
- additionfilled with H2
- filtrationAfter that time, the mixture was filtered
- concentrationconcentrated in vacuo