反应详情

To a solution of 1,1-dimethylethyl[(4-{[3-{[(5-chloro-2-thienyl)sulfonyl]amino}-4-(methyloxy)-1H-indazol-1-yl]methyl}phenyl)methyl]carbamate (for a preparation see Intermediate 29) (92 mg, 0.16 mmol) in dichloromethane (3 mL) was added dropwise hydrogen chloride (0.041 mL, 0.163 mmol). The resulting mixture was stirred at room temperature for 4 h, and then additional portion of hydrogen chloride (0.041 mL, 0.163 mmol) was added dropwise and the mixture was stirred at room temperature overnight. The solvents were then evaporated in a nitrogen blowdown unit. The residue was dissolved in 1:1 MeOH-DMSO (1 mL) and purified by Mass Directed AutoPrep (supelcosil ABZ+Plus column) eluting with solvents NB (A: Water+0.1% Formic acid, B: MeCN:Water 95:5+0.05% Formic acid). The solvent was dried under a stream of nitrogen in the Radleys blowdown apparatus to give the title compound (69 mg, 83%). LCMS (System E) RT=2.10 min, ES+ve m/z 463/465 (M+H)+.

1. stirringthe mixture was stirred at room temperature overnight
2. customThe solvents were then evaporated in a nitrogen
3. dissolutionThe residue was dissolved in 1:1 MeOH-DMSO (1 mL)
4. custompurified by Mass Directed AutoPrep (supelcosil ABZ+Plus column)
5. washeluting with solvents NB (A: Water+0.1% Formic acid, B
6. customThe solvent was dried under a stream of nitrogen in the Radleys blowdown apparatus