HRID520441

反应详情

EQUATION

反应方程式

HRID 520441 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

8-nitro-2-(3-(trifluoromethyl)phenyl)-4H-benzo[d][1,3]oxazin-4-one 3 (150 mg, 0.45 mmol) was added to a solution of ammonia (5.0 mL, 10 mmol) in IPA. The reaction mixture was heated under gentle reflux for 12 h then cooled to room temperature. The reaction mixture was poured into H2O and the resulting precipitate was collected by filtration rinsed with H2O and dried under vacuum. The crude residue was recrystallized from EtOAc to give 8 (91 mg, 62% yield) as a yellow solid.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureunder gentle reflux for 12 h
  3. filtrationthe resulting precipitate was collected by filtration
  4. washrinsed with H2O
  5. customdried under vacuum
  6. customThe crude residue was recrystallized from EtOAc