反应详情

To a solution of 5.5 mg (1RS,3SR)-6-(1,1-difluoro-methoxy)-1-(3-hydroxy-phenyl)-3-methyl-2,3,4,9-tetrahydro-1H-beta-carboline-3-carboxylic acid methyl ester in 10 ml 2-butanon are added 132 μl bromoethyl isocyanate. The mixture is heated to reflux for 30 h. An aqueous solution of sodium bicarbonate is added and the mixture is extracted with ethyl acetate. The organic layer is washed with brine and dried with magnesium sulfate. The solvent is removed at reduced pressure. After column chromatography (silica gel; toluene, ethyl acetate 4:1) and trituration with diisopropylether, 550 mg (61%) of the title compound are obtained as a colorless solid. MS: m/z (MH+)=519.9/522.0

1. temperatureThe mixture is heated
2. temperatureto reflux for 30 h
3. extractionthe mixture is extracted with ethyl acetate
4. washThe organic layer is washed with brine
5. dry with materialdried with magnesium sulfate
6. customThe solvent is removed at reduced pressure