HRID221766

反应详情

EQUATION

反应方程式

HRID 221766 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 5-(2-fluoro-phenyl)-5-trifluoromethyl-2,5,6,7-tetrahydro-[1,4]oxazepin-3-ylamine (1.12 g, 4.05 mmol) in 12 mL concentrated sulfuric acid (95%) was added potassium nitrate (533 mg, 5.27 mmol) in two portions. The reaction mixture was stirred at rt for 30 minutes, it was then poured onto ice water and TBME was added. The layers were separated, washed with water and TBME. The combined aqueous layers were basified with solid Na2CO3 and extracted with EtOAc. The EtOAc layers were dried over MgSO4.H2O and evaporated to give 1.29 g of the title compound was a white solid.

WORKUP

后处理

  1. additionwas added
  2. customThe layers were separated
  3. washwashed with water and TBME
  4. extractionextracted with EtOAc
  5. dry with materialThe EtOAc layers were dried over MgSO4.H2O
  6. customevaporated