HRID1197765

反应详情

EQUATION

反应方程式

HRID 1197765 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a suspension of 0.50 g 2-(7-acetamido-3,4-dihydro-2,2-dimethyl-6-nitro-2H-1,4-benzoxazin-4-yl)pyridine N-oxide in 6 ml ethanol, was added 6 ml of 5N HCl, the mixture was stirred at 100° C. for two hours, the reaction mixture was poured to ice water, and the resulting mixture was neutralized with sodium bicarbonate and extracted with chloroform. The extract was dried over anhydrous magnesium sulfate, the solvents were distilled off from the dried solution, and the residue thus obtained was recrystallized from ethanol, thus giving 359 mg of 2-(7-amino-3,4-dihydro-2,2-dimethyl-6-nitro-2H-1,4-benzoxazin-4-yl)pyridine N-oxide.

WORKUP

后处理

  1. extractionextracted with chloroform
  2. dry with materialThe extract was dried over anhydrous magnesium sulfate
  3. distillationthe solvents were distilled off from the dried solution
  4. customthe residue thus obtained
  5. customwas recrystallized from ethanol