HRID619737
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
- 100 °C
PROCEDURE
实验过程
To a DMF solution 15 ml of 5-fluoro-6-nitrobenzoimidazolinone 500 mg (2.5 mmol) and 5-isoquinolinethiol 450 mg (2.8 mmol), potassium carbonate 550 mg (4.0 mmol) was added, and the mixture was heated with stirring for 2 hours at 100° C. After adding water, the reaction mixture was extracted with ethyl acetate. The organic layer was washed with a saturated water solution of sodium chloride, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was crystallized from methanol, and 5-(5-isoquinolylsulfanyl)-6-nitro-2,3-dihydro-1H-benzo[d]imidazol-2-one 346 mg (40.3%) was obtained.
WORKUP
后处理
- temperaturethe mixture was heated
- extractionthe reaction mixture was extracted with ethyl acetate
- washThe organic layer was washed with a saturated water solution of sodium chloride
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was crystallized from methanol