HRID23648
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 121 mg of compound N-(4-chlorobenzyl)-2-{[[(2R)-2-(2-furyl)-2-hydroxyethyl](methyl)amino]methyl}-4-methyl-7-oxo-3-{[2-(trimethylsilyl)ethoxy]methyl}-4,7-dihydrothieno[3,2-b]pyridine-6-carboxamide in 3 mL of 75% TFA in CH2Cl2 is stirred at room temperature for 3 h, then diluted with CHCl3 and added to stirred aq. NaHCO3. The aqueous phase is extracted with 4 portions of CH2Cl2, and the combined organic phases dried (Na2SO4) and concentrated under reduced pressure. Flash chromatography of the residue on silica gel using 3% MeOH in CH2Cl2 provides 19 mg of the title compound as a brown solid. Recrystallization from EtOAc-hexane affords granular brown crystals.
WORKUP
后处理
- additionadded
- extractionThe aqueous phase is extracted with 4 portions of CH2Cl2
- dry with materialthe combined organic phases dried (Na2SO4)
- concentrationconcentrated under reduced pressure