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
N-(5-{(1R)-1-{[tert-butyl(dimethyl)silyl]oxy}-2-[(8-{3-[(1R)-3-(diisopropylamino)-1-phenylpropyl]-4-hydroxyphenyl}octyl)amino]ethyl}-2-hydroxyphenyl)methanesulfonamide (Preparation 55, 74 mg, 0.095 mmol) was dissolved in tetrahydrofuran (3 ml) and triethylaminetrihydrofluoride (90 ul, 0.54 mmol) was added in one portion at room temperature. The reaction was stirred for 12 hours and the solvent removed under reduced pressure, the residue was dissolved in methanol (10 ml) and 880 ammonia (1 ml) and the solvent removed under reduced pressure. The residue was purified by column chromatography on silica gel eluting with dichloromethane:methanol:880 ammonia (97/3/0.3 to 85/15/1.5 by volume) to furnish the title compound as a yellow solid, 34 mg.
WORKUP
后处理
- customthe solvent removed under reduced pressure
- dissolutionthe residue was dissolved in methanol (10 ml)
- custom880 ammonia (1 ml) and the solvent removed under reduced pressure
- customThe residue was purified by column chromatography on silica gel eluting with dichloromethane