反应 #1352574
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08772323B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 40 mg (119 μmol) 5-ethyl-6-[2-(4-hydroxy-phenyl)-benzoxazol-6-yl]-4,5-dihydro-2H-pyridazin-3-one, 23.5 mg (128 μmol) 1-(2-chloro-1-methylethyl)pyrrolidine×HCl, 50 mg (362 μmol) potassium carbonate and 2 ml DMF are heated together for 6 h to 80° C. Then the mixture is extracted with 10% sodium carbonate solution and EA. The org. phase is washed with sat. saline solution, dried on sodium sulphate and then the solv. is totally eliminated i.V. The residue is separated by semipreparative HPLC-MS. (xBridge, MeOH/H2O+TFA) Then the mixture is extracted with 10% sodium carbonate solution and EA phase is washed with sat. saline solution dried on sodium sulphate The residue is separated by semipreparative HPLC-MS
来源 ID: ord-6fdda7cbdd5443b9b01588bd72605128