反应详情

温度

70 °C

Ethanolamine (0.320 mL, 5.30 mmol) was added to a solution of 10-(5-chlorofuran-2-yl)-8-((1,3-dioxoisoindolin-2-yl)methyl)-1,3-dimethyl-5-(4-methylthiazol-2-yl)-7,8-dihydro-1H-pyrimido[4′,5′:3,4]pyrrolo[2,1-c][1,4]thiazine-2,4(3H,10H)-dione (537 mg, 0.883 mmol) in toluene (10 mL). The mixture was stirred at 70° C. for 3 hours and then cooled to room temperature for 16, then heated at 70° C. for a further 2.5 hours and again cooled to room temperature. The mixture was diluted with water (100 ml) and ethyl acetate (100 ml). The organic phase was separated, washed with 1M NaOH(aq) (50 ml) passed through a hydrophobic frit and evaporated under vacuum to afford the title compound as a mixture of diastereomers.

1. temperaturecooled to room temperature for 16
2. temperatureheated at 70° C. for a further 2.5 hours
3. temperatureagain cooled to room temperature
4. customThe organic phase was separated
5. washwashed with 1M NaOH(aq) (50 ml)
6. customevaporated under vacuum