HRID1727254
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- concentrationThe reaction mixture was concentrated
- dissolutionthe residue was dissolved in 1 N HCl aqueous solution (pH 5)
- customThe solid precipitated
- filtrationwas collected by filtration
- customdried under vacuum
- customcrystallized from MeOH/CH2Cl2/ether