HRID561177

反应详情

EQUATION

反应方程式

HRID 561177 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of ethyl (3R)-8-amino-9,10-difluoro-3-fluoromethyl-2,3-dihydro-7-oxo-7H-pyrido[1,2,3-de]-1,4-benzoxazine-6-carboxylate (270 mg, 0.789 mmol) in a mixture of H2SO4—H2O—AcOH (1:5:6, 3 mL) was heated under reflux for 1 h. The reaction mixture was poured into ice-water and the resulting precipitates were collected by filtration. The filtered precipitates were washed with water, and dried in vacuo to give (3R)-8-amino-9,10-difluoro-3-fluoromethyl-2,3-dihydro-7-oxo-7H-pyrido[1,2,3-de]-1,4-benzoxazine-6-carboxylic acid (237 mg, 96%) as a yellow powder.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 1 h
  3. customthe resulting precipitates
  4. filtrationwere collected by filtration
  5. customThe filtered precipitates
  6. washwere washed with water
  7. customdried in vacuo