反应详情

A cooled (0° C.) brown solution of (rac)-6-(8-amino-5,6,7,8-tetrahydroisoquinolin-4-yl)-1-methyl-3,4-dihydroquinolin-2(1H)-one (intermediate A-2) (61.5 mg, 200 μmol) in CH2Cl2 (3.0 ml) was treated with ethanesulfonyl chloride (65.6 mg, 48.3 μL, 500 μmol) and Et3N (40.5 mg, 55.8 μL, 400 μmol). After ½ h the mixture was concentrated in vacuo and purified by flash chromatography (20 g SiO2, Telos-cartridge, CH2Cl2/MeOH (1 to 5%)) to give 100 mg of the title compound together with Et3N×HCl as impurity. Extraction with H2O/EtOAc (3×), and precipitation CH2Cl2/n-pentane gave the pure title compound (46 mg, 58%) as a yellow powder. MS: 400.2 (M+H+).

1. concentrationAfter ½ h the mixture was concentrated in vacuo
2. custompurified by flash chromatography (20 g SiO2, Telos-cartridge, CH2Cl2/MeOH (1 to 5%))