HRID1719692
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
A mixture of about 9.0 g of 1H-1,2,4-triazole, about 6.24 g of approximately 50% sodium hydride in oil and about 130 ml of dimethylformamide was stirred for about 1.5 hours, then about 33 g of bromobutylphthalimide was added and this mixture was heated on a steam bath for about 6 hours, then concentrated to a solid residue. Water and methylene chloride were added, the organic layer was separated, washed with water, dried and concentrated to a residue. This residue was recrystallized from ethanol, giving about 27.3 g of 2-[4-(1H-1,2,4-triazol-1-yl)butyl]-1H-isoindol-1,3(2H)-dione.
WORKUP
后处理
- temperaturethis mixture was heated on a steam bath for about 6 hours
- concentrationconcentrated to a solid residue
- additionWater and methylene chloride were added
- customthe organic layer was separated
- washwashed with water
- customdried
- concentrationconcentrated to a residue
- customThis residue was recrystallized from ethanol