HRID1723685

反应详情

EQUATION

反应方程式

HRID 1723685 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture solution of 8-(2-chlorophenylamino)-6,7-difluoro-4-methyl-benzo[d][1,2]oxazin-1-one (26 mg, 0.079 mmol) and Zn (30 mg, 0.46 mmol) in AcOH (2 mL) was heated for 1 hour at 85° C. The reaction mixture was filtered and the solid was washed with additional AcOH. The filtrate was concentrated in vacuo, diluted with EtOAc, and washed with saturated aqueous NaHCO3 and water. The organic layer was dried over MgSO4, filtered, and concentrated in vacuo to give the desired product (18 mg, 74%) that was used directly without further purification.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered
  2. washthe solid was washed with additional AcOH
  3. concentrationThe filtrate was concentrated in vacuo
  4. additiondiluted with EtOAc
  5. washwashed with saturated aqueous NaHCO3 and water
  6. dry with materialThe organic layer was dried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo