HRID64850

反应详情

EQUATION

反应方程式

HRID 64850 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 9.0 g of 1H-1,2,4-triazole, 6.24 g of approximately 50% sodium hydride in oil and 130 ml of dimethylformamide was stirred for 1.5 hours, then 33 g of N-(4-bromobutyl)phthalimide was added and this mixture was heated on a steam bath for 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 27.3 g of 2-[4-(1H-1,2,4-triazol-1-yl)butyl]-1H-isoindol-1,3(2H)-dione.

WORKUP

后处理

  1. temperaturethis mixture was heated on a steam bath for 6 hours
  2. concentrationconcentrated to a solid residue
  3. additionWater and methylene chloride were added
  4. customthe organic layer was separated
  5. washwashed with water
  6. customdried
  7. concentrationconcentrated to a residue
  8. customThis residue was recrystallized from ethanol