HRID19419
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 {(S)-1-[1-(2-hydroxy-2-methyl-propyl)-1H-pyrazol-3-ylcarbamoyl]-3-methyl-butyl}-carbamic acid t-butyl ester (4.15 g) in dichloromethane (8 mL) was treated with trifluoroacetic acid (8 mL) and stirred at room temperature for 1 h. At this time the mixture was concentrated in vacuo and the residue dissolved in methanol (10 mL) and treated with hydrogen chloride gas for 2 min. The mixture was concentrated in vacuo and the residue was dried under high vacuum. The solid obtained was triturated with diethyl ether which afforded (S)-2-amino-4-methyl-pentanoic acid [1-(2-hydroxy-2-methyl-propyl)-1H-pyrazol-3-yl]amide hydrochloride (3.86 g, 100%) as a white solid.
WORKUP
后处理
- concentrationAt this time the mixture was concentrated in vacuo
- dissolutionthe residue dissolved in methanol (10 mL)
- additiontreated with hydrogen chloride gas for 2 min
- concentrationThe mixture was concentrated in vacuo
- customthe residue was dried under high vacuum
- customThe solid obtained
- customwas triturated with diethyl ether which