反应详情

To a solution of 2-(7-chloro-thieno[3,2-b]pyridin-2-yl)-5-(2-trimethylsilanyl-ethoxymethyl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid [(R)-2-(3-cyano-azetidin-1-yl)-1-cyclopropyl-2-oxo-ethyl]-amide (30 mg, 0.048 mmol) in dichloromethane (2 mL) was added trifluoroacetic acid (0.37 mL, 4.82 mmol). The reaction mixture was stirred for 3 h at room temperature then concentrated and dried under high vacuum for 1 h. The residue was dissolved in 3 mL of CH2Cl2:MeOH:NH4OH (80:19:1) and stirred at room temperature for 18 h then evaporated to dryness under vacuum. The crude residue was washed with MeOH (3×3 mL) to give 17 mg (72%) of 2-(7-chloro-thieno[3,2-b]pyridin-2-yl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid [(R)-2-(3-cyano-azetidin-1-yl)-1-cyclopropyl-2-oxo-ethyl]-amide. MS: (M+H)+=492.

1. concentrationthen concentrated
2. customdried under high vacuum for 1 h
3. dissolutionThe residue was dissolved in 3 mL of CH2Cl2:MeOH:NH4OH (80:19:1)
4. stirringstirred at room temperature for 18 h
5. customthen evaporated to dryness under vacuum
6. washThe crude residue was washed with MeOH (3×3 mL)