反应详情

To a solution of (5)-ethyl 2-(3-(2-chloro-5-fluoropyrimidin-4-ylamino)cyclohexylidene)ethanoate, 62a, (2.58 g, 8.22 mmol) in nitromethane (44.53 mL, 822.3 mmol) was added 1,1,3,3-tetramethylguanidine (1.55 mL, 12.33 mmol). The reaction was refluxed overnight then concentrated in vacuo and purified by silica gel chromatography (Hexanes:EtOAc) then a second chromatography (CH2Cl2:20% MeOH in CH2Cl2). Fractions containing pure product were combined and concentrated to give 1.8 g of 62b

1. temperatureThe reaction was refluxed overnight
2. concentrationthen concentrated in vacuo
3. custompurified by silica gel chromatography (Hexanes:EtOAc)
4. additionFractions containing pure product
5. concentrationconcentrated