HRID1898352
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
To a solution of methyl 2-[(2-chloro-6-fluorophenyl)amino]-6-hydroxy-7-nitro-1H-benzimidazole-5-carboxylate (Step-2 of Intermediate-56, 0.500 g) in benzene (2.0 mL), were added iron powder (0.500 g) and acetic acid (4.0 mL). The reaction mass was refluxed for 3 h. Decant the reaction mass removed the solvent under vacuum. The obtained solid mass was washed with water. The reaction mass was extracted with MeOH:DCM (5%). The organic layer was dried over anhydrous sodium sulphate and concentrated to afford 0.440 g of the desired product.
WORKUP
后处理
- temperatureThe reaction mass was refluxed for 3 h
- customDecant the reaction mass
- customremoved the solvent under vacuum
- washThe obtained solid mass was washed with water
- extractionThe reaction mass was extracted with MeOH
- dry with materialThe organic layer was dried over anhydrous sodium sulphate
- concentrationconcentrated