反应详情

To a solution of (S)-(4-(1-(4-(hydroxymethyl)phenyl)pyrido[3,4-d]pyridazin-4-yl)-2-methylpiperazin-1-yl)(piperidin-1-yl)methanone 9 (100 mg, 224 μmol) in chloroform (2 mL) was added 2,2,2-trichloroacetyl isocyanate (39 μl, 314 μmol). The reaction was stirred at RT for 1 h and deposited on 3 g of Alumina (Brockmann II). After 1 h, the product was eluted from the alumina with 10% MeOH in dichloromethane. The crude reaction product was concentrated and purified by column chromatography to afford (S)-(4-(4-(3-methyl-4-(piperidine-1-carbonyl)piperazin-1-yl)pyrido[3,4-d]pyridazin-1-yl)phenyl)methyl carbamate 10. MS 489.2 (calc'd) 490.1 (M+H, found).

1. waitAfter 1 h
2. washthe product was eluted from the alumina with 10% MeOH in dichloromethane
3. customThe crude reaction product
4. concentrationwas concentrated
5. custompurified by column chromatography