反应详情

4-cyano-3-(2,4-dichlorophenyl)-5-morpholin-4-ylthiophene-2-carboxylic acid (0.030 g, 0.08 mmol) was weighed out into a microwave tube that was then sealed. Toluene (1 ml), TEA (0.014 mL, 0.100 mmol) and diphenylphosphoryl azide (0.020 mL, 0.091 mmol) were added to the tube. The reaction mixture was shaken at room temperature for 30 minutes, and then heated to 80° C. for 2 hours. 2-aminoethanol (0.0061 ml, 0.1 mmol) and anhydrous THF (1 mL) and TEA (0.014 mL, 0.100 mmol) were pre-mixed and then added to the reaction mixture. The reaction was heated at 80° C. for a further 60 minutes, then allowed to cool to RT and shaken overnight. The solvent was evaporated in a Genevac HT12 and the residue was purified on the Agilent 100 series LC/MSD (FA) to give N-[4-cyano-3-(2,4-dichlorophenyl)-5-morpholin-4-yl-2-thienyl]-N-(2-hydroxyethyl)urea (86). LCMS: (FA) ES+ 441.3.

1. customthat was then sealed
2. temperatureheated to 80° C. for 2 hours
3. additionadded to the reaction mixture
4. temperatureThe reaction was heated at 80° C. for a further 60 minutes
5. temperatureto cool to RT
6. stirringshaken overnight
7. customThe solvent was evaporated in a Genevac HT12
8. customthe residue was purified on the Agilent 100 series LC/MSD (FA)