反应详情

温度

85 °C

To a solution of 4-(1-(2-chlorophenoxy)ethyl)-6-(methylthio)-1,3,5-triazin-2-amine (16a) (181 mg) in ethanol (10 mL) was added. Raney-nickel was added via a syringe (2.0 mL) and the reaction mixture was heated at 85° C. for 40 minutes then cooled to room temperature and the mixture was filtered over Celite and washed with ethanol/water (1/1 v/v) and methanol. The filtrate was concentrated in vacuo and further purified by column chromatography (eluting with 1% acetontrile in dichloromethane) to give the title compound (25 mg), MS (ES): m/z 251 [M+H]+.

1. temperaturethen cooled to room temperature
2. filtrationthe mixture was filtered over Celite
3. washwashed with ethanol/water (1/1 v/v) and methanol
4. concentrationThe filtrate was concentrated in vacuo
5. customfurther purified by column chromatography (eluting with 1% acetontrile in dichloromethane)