反应详情

温度

80 °C

To the reaction flask, tert-butyl 3-(5-(3-chlorophenylamino)-3-formylpyrazolo[1,5-a]pyrimidin-7-ylamino)benzoate (122 mg, 0.3 mmol) was added to ethanol (1.3 mL) along with hydantoin (26 mg, 0.3 mmol) and piperidine (26 μL, 0.3 mmol). The reaction was heated at 80° C. for 2 hours in the microwave then cooled to room temperature and diluted with water. The solid was collected by filtration, washed with water, 50% ethanol/water, and then 100% ethanol. The material was dried under vacuum overnight. The product, tert-butyl 3-(5-(3-chlorophenylamino)-3-((2,5-dioxoimidazolidin-4-ylidene)methyl)pyrazolo[1,5-a]pyrimidin-7-ylamino)benzoate, was recovered as a solid in 69% yield. LCMS (M+1=546)

1. temperaturethen cooled to room temperature
2. filtrationThe solid was collected by filtration
3. washwashed with water, 50% ethanol/water
4. customThe material was dried under vacuum overnight
5. customThe product, tert-butyl 3-(5-(3-chlorophenylamino)-3-((2,5-dioxoimidazolidin-4-ylidene)methyl)pyrazolo[1,5-a]pyrimidin-7-ylamino)benzoate, was recovered as a solid in 69% yield