反应详情

温度

65 °C

To a solution of N-(3-(5-amino-1-tosyl-1H-pyrrolo[2,3-b]pyridin-4-ylamino)-4-ethylcyclopentyl)cyclopropanesulfonamide (0.095 g, 75% purity, 0.142 mmol, prepared using L from Preparation #27 and Preparation #000.1 with DIEA, K.1 with TsCl and NaH, and BBB) and TMOF (0.016 mL, 0.147 mmol) in MeOH (3.09 mL) was added toluene-4-sulfonic acid hydrate (0.0003 g, 0.0015 mmol). The reaction was heated at about 65° C. for about 14 h. The reaction was cooled to ambient temperature and concd under reduced pressure to give a crude solid. The solid was dissolved in EtOAc (10 mL) and was washed with saturated aqueous NaHCO3 (5 mL), water (5 mL), and brine (5 mL). The organic portion was separated and dried over anhydrous MgSO4, filtered, and concd under reduced pressure to afford N-(3-ethyl-4-(6-tosylimidazo[4,5-d]pyrrolo[2,3-b]pyridin-1(6H)-yl)cyclopentyl)cyclopropanesulfonamide (0.075 g, 99%) as a yellow solid: LC/MS (Table 1, Method a) Rt=2.15 min; MS m/z: 514 (M+H)+.

1. temperatureThe reaction was cooled to ambient temperature
2. customconcd under reduced pressure to give a crude solid
3. washwas washed with saturated aqueous NaHCO3 (5 mL), water (5 mL), and brine (5 mL)
4. customThe organic portion was separated
5. dry with materialdried over anhydrous MgSO4
6. filtrationfiltered