反应详情

温度

45 °C

4-Chloro-1-isocyanato-2-methyl-benzene (93.3 mg, 0.56 mmol) was added to a solution of (4-Amino-7-isopropyl-7H-pyrrolo[2,3-d]pyrimidin-5-yl)-(5-amino-pyridin-3-yl)-methanone (150 mg, 0.51 mmol) in pyridine (5 mL). The mixture was heated to 45° C. for 12 h. The reaction mixture was concentrated in vacuo and the resulting yellow solid was triturated with CH2Cl2, filtered, and washed with CH2Cl2. Purification by flash column chromatography [(10% NH4OH/MeOH)/ethyl acetate 2:98] afforded the title compound as a white solid (197 mg, 83%). MS: 464.1 (MH+); HPLC Rf: 5.55 min. (HPLC method 4).

1. concentrationThe reaction mixture was concentrated in vacuo
2. customthe resulting yellow solid was triturated with CH2Cl2
3. filtrationfiltered
4. washwashed with CH2Cl2
5. customPurification by flash column chromatography [(10% NH4OH/MeOH)/ethyl acetate 2:98]