反应详情

Fe (8.24 g, 147.55 mmol) was added to a solution of (4-Amino-7-cyclopentyl-7H-pyrrolo[2,3-d]pyrimidin-5-yl)-(3-nitro-phenyl)methanone (10.37 g, 29.51 mmol) and NH4Cl (6.31 g, 118.0 mmol) in 1,4-Dioxane (200 mL), EtOH (150 mL), and water (100 mL). The resulting suspension was heated to reflux for 2 h, at this time the reaction was cooled to room temperature then filtered through celite eluting with EtOAc. The filtrate was dried over MgSO4 and concentrated to afford the title compound as a yellow solid (9.48 g, 100%). MS: 322.3 (MH+); HPLC Rf: 4.55 min. (HPLC method 4).

1. temperatureThe resulting suspension was heated
2. temperatureto reflux for 2 h, at this time the reaction
3. filtrationthen filtered through celite
4. washeluting with EtOAc
5. dry with materialThe filtrate was dried over MgSO4
6. concentrationconcentrated