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
To a 0° C. suspension of MeNH2.HCl (97.9 mg, 1.45 mmol) in benzene (4 ml) was added Me3Al (2 M in toluene, 746 μl, 1.45 mmol). The mixture was stirred for 5 minutes and at room temperature for about 1.25 hours. A suspension of 3-(1H-indol-6-yl)-3-(1H-indol-3-yl)-propionic acid ethyl ester XXVII in benzene (15 ml) was added, and the resulting reaction mixture was stirred at reflux for 8 hours, and at room temperature for 16 hours. The reaction mixture was diluted with a saturated solution of NH4Cl (20 ml) and extracted with EtOAc. The organic layers were combined, dried over Na2SO4, filtered, concentrated, and purified via flash chromatography (DCM/MeOH) affording 3-(1H-Indol-6-yl)-3-(1H-indol-3-yl)-N-methyl-propionamide XXVIII as a yellow oil (86 mg).
WORKUP
后处理
- additionwas added
- customthe resulting reaction mixture
- stirringwas stirred
- temperatureat reflux for 8 hours
- waitat room temperature for 16 hours
- extractionextracted with EtOAc
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- custompurified via flash chromatography (DCM/MeOH)