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, 19 μL (241 μmol) 2-methoxyethanol, 66 mg (251 μmol) diphenyl-2-pyridylphosphine and 10 ml THF are placed under protective gas. At 0° C. 58 mg (252 μmol) 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 20 mL of 4N HCl for 5 min and then extracted. The organic phase is washed with saturated saline solution and then the solv. is eliminated i.V. The residue is purified on silica gel. (Eluant: DCM/MeOH/ammonia) The solv. of the corresponding fractions is eliminated i.V. and the residue is crystallised with cyclohexane/EA.

1. customAt 0° C
2. extractionextracted with 10% sodium carbonate solution
3. stirringThe organic phase is stirred with 20 mL of 4N HCl for 5 min
4. extractionextracted
5. washThe organic phase is washed with saturated saline solution
6. customThe residue is purified on silica gel
7. customand the residue is crystallised with cyclohexane/EA