反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A solution of 1.499 g of ethyl[4-[2-[2-hydroxy-5-(N-hydroxycarbamimidoyl)benzenesulfonylamino]ethyl]-2′-methane sulfonylbiphenyl-3-yloxy]acetate in 20 mL of 34% hydrogen chloride/n-butanol solution was stirred at 60° C. for 3 hours. The reaction mixture was concentrated under a reduced pressure, and the crude crystals were recrystallized from n-butanol/diisopropyl ether to give 1.472 g of n-butyl [4-[2-[2-hydroxy-5-(N-hydroxycarbamimidoyl)benzenesulfonyl amino]ethyl]-2′-methanesulfonylbiphenyl-3-yloxy]acetate hydrochloride as a white crystal. The crystals thus obtained were identified as crystalline form A by an X-ray powder diffraction analysis. An X-ray powder diffraction pattern of the crystals was shown in FIG. 3.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated under a reduced pressure
- customthe crude crystals were recrystallized from n-butanol/diisopropyl ether