反应 #1858074
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07435744B2
反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a mixture of 0.3g (1.5 mmol) of N-(2-oxo-2,3-dihydro-benzoxazol-6-yl)-oxalamic acid, 0.165 ml (1.5 mmol) of N-methyl-morpholine in 8 ml of dimethylformamid 0.2 ml (1.5 mmol) of isobutyl-chloroformate is added dropwise at 0° C. and the mixture is stirred at 0° C. for 1 hour. Then 0.333 g (1.4 mmol) of 4-piperidin-4-ylmethyl-benzonitrile hydrochloride and 0.165 ml (1.5 mmol) of N-methyl-morpholine are added and the reaction mixture is stirred at 0° C. for 1 hour, at room temperature for 16 hours. The reaction mixture is concentrated and the residue is purified by column chromatography using Kieselgel 60 (Merck) as adsorbent and toluene:methanol=4:1 as eluent to yield 0.045 g (8.0%) of the title compound. Rf.: 0.4. Melting Point: 259-260° C. (isopropanol). is added dropwise at 0° C. the reaction mixture is stirred at 0° C. for 1 hour, at room temperature for 16 hours The reaction mixture is concentrated the residue is purified by column chromatography
来源 ID: ord-a114bd94bb0d425ebe3d57a283900bfe