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
CONDITIONS
反应条件
- 温度
- 140 °C
PROCEDURE
实验过程
A mixture containing 2-(3-isopropyl-2-oxo-2,3-dihydro-benzoimidazol-1-ylmethyl)-1-(3-methyl-butyl)-1H-benzoimidazole-5-carbonitrile (152 mg, 0.379 mmol), hydroxylamine hydrochloride (95 mg, 1.36 mmole) and potassium carbonate (105 mg, 0.758 mmole) in ethanol (4 mL) and water (2 mL) in a sealed tube was placed in a microwave oven (Smith Creator, Personal Chemistry) and heated at 140° C. for 15 min, followed by 150° C. for 10 min while stirring. The solvents were removed in vacuo and the residue was triturated with water. The white precipitate was collected by filtration, washed with water and dried in vacuo to give N-hydroxy-2-(3-isopropyl-2-oxo-2,3-dihydro-benzoimidazol-1-ylmethyl)-1-(3-methyl-butyl)-1H-benzoimidazole-5-carboxamidine (140 mg, 85%) as a white solid:
WORKUP
后处理
- customwas placed in a microwave oven
- customThe solvents were removed in vacuo
- customthe residue was triturated with water
- filtrationThe white precipitate was collected by filtration
- washwashed with water
- customdried in vacuo