反应 #1792722
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07329668B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A vial was charged with 2-Methyl-3-oxo-3-phenyl-propionitrile (1.0 g, 6.28 mmol), hydrazine (0.2 mL) and EtOH (1 mL), and subject to microwave irradiation at 100° C. for 50 min. Flach chromatography of the crude product using 3%-5% MeOH in CH2Cl2 gave the pyrazolylamine as a yellow oil (0.21 g). LC/MS (10% MeOH, 90% H20, 0.2% H3PO4 to 90% MeOH, 10% H20, 0.2% H3PO4, 2 minute gradient with an Exterra C18 S-5 column 4.6×30 mm): [M+H]+ m/z=174.10; retention time=1.02 min. irradiation at 100° C. for 50 min
来源 ID: ord-d5c9439af1874c06a5b7a5a8f7302d9e