反应详情

In a 10 mL round-bottomed flask, 2-cyclopropyl-5-(2-trimethylsilanyl-ethoxymethyl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid (1-methanesulfonyl-pyrrolidin-3-yl)-amide (177 mg, 0.37 mmol) was dissolved in CH2Cl2 (3 mL). Trifluoroacetic acid (1.1 mL) was added and the light yellow reaction mixture was stirred at room temperature for 2 h then concentrated. The residue was taken up in toluene (5 mL), concentrated and then dried under high vacuum. The residue was dissolved in CH2Cl2 (2.5 mL) and ethylenediamine (1.5 mL) was added. The reaction mixture was stirred at room temperature overnight then diluted with MeOH and the solid precipitate was collected via filtration. The solid residue was rinsed with hot water and EtOAc then dried under high vacuum to afford 56 mg (43%) of 2-cyclopropyl-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid (1-methanesulfonyl-pyrrolidin-3-yl)-amide as a white solid. MS: (M+H)+=350; mp>300.

1. concentrationthen concentrated
2. concentrationconcentrated
3. customdried under high vacuum
4. dissolutionThe residue was dissolved in CH2Cl2 (2.5 mL)
5. additionethylenediamine (1.5 mL) was added
6. stirringThe reaction mixture was stirred at room temperature overnight
7. additionthen diluted with MeOH
8. filtrationthe solid precipitate was collected via filtration
9. washThe solid residue was rinsed with hot water and EtOAc
10. customthen dried under high vacuum