反应详情

温度

-78 °C

A solution of 150 mg (3aSR,10RS)-2-(2-dimethylamino-ethyl)-10-(3-hydroxy-phenyl)-6-methoxy-3a-methyl-3a,4,9,10-tetrahydro-2,9,10a-triaza-cyclopenta[b]fluorene-1,3-dione (example 7) in 5 ml dichloromethane is cooled to −78° C. 20 ml bor tribromide are added drop wise. The suspension is stirred for 30 min at −78° C. and allowed to warm up to room temperature. After stirring for 1 h at room temperature, the mixture is cooled to 0° C. and an aqueous solution of sodium bicarbonate is added. The organic layer is separated and dried with magnesium sulfate. The solvent is removed at reduced pressure. After column chromatography (silica gel, ethyl acetate, methanol, ammonia 10:0.3:0.2), 49 mg of the title compound are obtained as a colourless foam. MS: m/z (MH+)=435.2

1. additionare added drop wise
2. temperatureto warm up to room temperature
3. stirringAfter stirring for 1 h at room temperature
4. temperaturethe mixture is cooled to 0° C.
5. customThe organic layer is separated
6. dry with materialdried with magnesium sulfate
7. customThe solvent is removed at reduced pressure