反应详情

温度

60 °C

Sodium Tungstate Dihydrate (62 mg, 0.19 mmol) and 7-(2-Methoxy-phenyl)-2-methylsulfanyl-pyrrolo[2,1-f][1,2,4]triazine (1.02 g, 3.76 mmol) were combined in Methanol (40.0 mL) and 50% Hydrogen Peroxide (0.65 mL, 11 mmol) was added and the reaction was stirred under an atmosphere of nitrogen at 60° C. for 5 h. The mixture was treated with 5 mL 10% Na2S2O3, generating a ppt, then allowed to cool to rt before being stored in a freezer for 30 min. The resultant solids were collected on a Buchner, washing with water (25 mL). Further drying in vacuo afforded 2-Methanesulfonyl-7-(2-methoxy-phenyl)-pyrrolo[2,1-f][1,2,4]triazine (1.00 g; Yield=87.7%). 1H-NMR (DMSO-d6): 9.38 (s, 1H), 7.75 (dd, 1H, J=1.6, 7.6 Hz), 7.51 (m, 2H), 7.40 (d, 1H, J=4.7 Hz), 7.25 (d, 1H, J=8.3 Hz), 7.13 (m, 1H), 3.83 (s, 3H), 3.37 (s, 3H).

1. temperatureto cool to rt
2. waitbefore being stored in a freezer for 30 min
3. customThe resultant solids were collected on a Buchner
4. washwashing with water (25 mL)
5. customFurther drying in vacuo