反应详情

温度

80 °C

Ethyl 2-benzimidazol-2-ylacetate (1.1 equivalents) and 2-amino-5-(4-methylpiperazinyl)benzenecarbonitrile (1.0 equivalent) were dissolved in 1,2-dichloroethane, and then SnCl4 (11 equivalents) was added. The mixture was heated at reflux overnight. Upon cooling, the mixture was concentrated in vacuo. NaOH (3 M) was added to the solid, and the mixture heated at 80° C. for 0.5 hours. The solid was filtered and washed sequentially with H2O, CH2Cl2, and acetone. LC/MS indicated that the product was present in the acetone layer and the solid. These fractions were combined and purified by silica gel chromatography (5-10% MeOH in CH2Cl2 with 1% Et3N) to give the desired product. LC/MS m/z 375.4 (MH+), Rt 1.65 minutes.

1. temperatureThe mixture was heated
2. temperatureat reflux overnight
3. temperatureUpon cooling
4. concentrationthe mixture was concentrated in vacuo
5. additionNaOH (3 M) was added to the solid
6. filtrationThe solid was filtered
7. washwashed sequentially with H2O, CH2Cl2, and acetone
8. custompurified by silica gel chromatography (5-10% MeOH in CH2Cl2 with 1% Et3N)