HRID1733698

反应详情

EQUATION

反应方程式

HRID 1733698 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 1 N aqueous sodium hydroxide (45 ml) is dissolved 1-hydroxy-6-nitro-1,2,3-benzotriazole (7.2 g). To the solution is added dropwise benzenesulfonyl chloride (7.0 g) with stirring at room temperature and further are added thereto water (50 ml) and ethyl acetate (100 ml) and the mixture is stirred for 1 hour. The ethyl acetate layer is separated, dried over magnesium sulfate-charcoal, filtered and concentrated until it becomes about 30 ml. n-Hexane (50 ml) is thereto added and the mixture is allowed to stand. The precipitated crystals are separated by filtration and dried to give faint yellow prisms of 1-benzenesulfonyloxy-6-nitro-1,2,3-benzotriazole (6.8 g), melting point: 122°-124° C. The product is recrystallized from ethyl acetate-n-hexane to give a pure product: melting point: 124° C.

WORKUP

后处理

  1. additionfurther are added
  2. customThe ethyl acetate layer is separated
  3. dry with materialdried over magnesium sulfate-charcoal
  4. filtrationfiltered
  5. concentrationconcentrated until it
  6. additionn-Hexane (50 ml) is thereto added
  7. customThe precipitated crystals are separated by filtration
  8. customdried