HRID982706
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 mixture of N-(4-chlorobenzyl)-2-iodo-4-methyl-7-oxo-4,7-dihydrothieno[3,2-b]pyridine-6-carboxamide (0.20 g, 0.44 mmol), Pd(PhCN)2Cl2 (10 mg) CuI (7 mg) Et3N (1 mL) and propargyl alcohol (0.036 g, 0.66 mmol) in DMF was stirred at ambient temperature overnight. The solvent was removed and the residue partitioned between H2O and CH2Cl2 (100 mL each). The layers were shaken, the organic layer separated and dried over MgSO4. The solvents were removed in vacuo and the residue purified via flash column chromatography (eluant 5% MeOH/CH2Cl2) to afford 0.117 g title compound as a white solid.
WORKUP
后处理
- customThe solvent was removed
- customthe residue partitioned between H2O and CH2Cl2 (100 mL each)
- stirringThe layers were shaken
- customthe organic layer separated
- dry with materialdried over MgSO4
- customThe solvents were removed in vacuo
- customthe residue purified via flash column chromatography (eluant 5% MeOH/CH2Cl2)