HRID1727254

反应详情

EQUATION

反应方程式

HRID 1727254 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 1.76 M NH2OH in MeOH (1.23 mL) was added the compound (150 mg, 0.31 mmol) from the process (1-2), and the mixture was stirred at room temperature for 24 hours. The reaction mixture was concentrated, and the residue was dissolved in 1 N HCl aqueous solution (pH 5). The solid precipitated was collected by filtration, dried under vacuum, and crystallized from MeOH/CH2Cl2/ether to afford the titled compound (67 mg, 46%) as a pale brown solid.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. dissolutionthe residue was dissolved in 1 N HCl aqueous solution (pH 5)
  3. customThe solid precipitated
  4. filtrationwas collected by filtration
  5. customdried under vacuum
  6. customcrystallized from MeOH/CH2Cl2/ether