反应详情

To a stirred solution of N-tert-butyl-2-(5-chloro-1H-indazol-1-yl)-5-((2-(trimethylsilyl)ethoxy)methyl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxamide (144 mg, 289 μmol) in dichloromethane (3 mL) was added trifluoroacetic acid (1 mL). After 15 h then mixture was concentrated in vacuo then 25 mL Jan. 10, 1960 of a mixture of ammonium hydroxide/methanol/dichloromethane added. After 1 h the mixture was concentrated in vacuo. Purification by chromatography (silica, 24 g Analogix column, 0-5% of a solution of methanol containing 10% ammonium hydroxide in dichloromethane) gave 2-(5-chloro-indazol-1-yl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid tert-butylamide (40.9 mg, 38%). MS (M+H)+=369; 1H NMR (DMSO-d6) δ: 9.02 (s, 1H), 8.60 (s, 1H), 8.57 (s, 1H), 8.53 (s, 1H), 8.43 (s, 1H), 8.09 (s, 1H), 7.61 (s, 1H), 1.50 (s, 9H).

1. concentrationmixture was concentrated in vacuo
2. addition10, 1960 of a mixture of ammonium hydroxide/methanol/dichloromethane
3. additionadded
4. concentrationAfter 1 h the mixture was concentrated in vacuo
5. customPurification by chromatography (silica, 24 g Analogix column, 0-5% of a solution of methanol containing 10% ammonium hydroxide in dichloromethane)