反应详情

40 mg (119 μmol) 5-ethyl-6-[2-(4-hydroxy-phenyl)-benzoxazol-6-yl]-4,5-dihydro-2H-pyridazin-3-one, 31 mg (238 μmol) 2-(ethyl-isopropyl-amino)-ethanol, 66 mg (251 μmol) triphenylphosphine and 5 ml THF are placed under protective gas. At 0° C., 58 mg (251 μmol) of DBAD are added and then the mixture is stirred overnight at RT. Then it is diluted with EA and extracted with 10% sodium carbonate solution. The organic phase is stirred with 15 mL of 4N HCl for 5 min and then extracted twice with diethyl ether. The acid H2O phase is made basic with sodium carbonate solution and extracted 3 times with DCM. The organic phase is washed with saturated saline solution and then the solv. is eliminated i.V. The residue is recrystallised with cyclohexane/EA.

1. extractionextracted with 10% sodium carbonate solution
2. stirringThe organic phase is stirred with 15 mL of 4N HCl for 5 min
3. extractionextracted twice with diethyl ether
4. extractionextracted 3 times with DCM
5. washThe organic phase is washed with saturated saline solution
6. customThe residue is recrystallised with cyclohexane/EA