反应详情

359 mg (1.137 mmol, 76% purity) of the compound from Example 23A are initially charged in 0.63 ml (8.64 mmol) of thionyl chloride. The reaction mixture is stirred at RT for 48 h. After concentration on a rotary evaporator, the residue is taken up in 10 ml of ethyl acetate and washed once with 5 ml of sat. aqueous sodium bicarbonate solution. The organic phase is dried over magnesium sulfate. After filtration, the solvent is removed on a rotary evaporator. The residue is purified by column chromatography on silica gel 60 (mobile phase gradient: cyclohexane/ethyl acetate 400:1→60:1). This gives a light-brown solid.

1. concentrationAfter concentration
2. customon a rotary evaporator
3. washwashed once with 5 ml of sat. aqueous sodium bicarbonate solution
4. dry with materialThe organic phase is dried over magnesium sulfate
5. filtrationAfter filtration
6. customthe solvent is removed on a rotary evaporator
7. customThe residue is purified by column chromatography on silica gel 60 (mobile phase gradient: cyclohexane/ethyl acetate 400:1→60:1)
8. customThis gives a light-brown solid