HRID369948
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 10-methyl-2,3-dihydro-1H-pyrrolo[2,1-c][1,4]benzodiazapine-5,11(10H,11aH)-dione (5.7 g, 24.7 mmol) in concentrated sulfuric acid (60 ml) at 0° C. was added potassium nitrate (2.62 g, 25.9 mmol). After stirring for 2 h the mixture was dumped onto ice (500 g) and extracted with ethyl acetate (5×75 ml). The combined extracts were washed with water, dried over magnesium sulfate, filtered, and concentrated to a solid which was recrystallized from ethyl acetate-hexane (5.2 g, 77%), m.p. 160-162° C.
WORKUP
后处理
- extractionextracted with ethyl acetate (5×75 ml)
- washThe combined extracts were washed with water
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated to a solid which
- customwas recrystallized from ethyl acetate-hexane (5.2 g, 77%), m.p. 160-162° C.