反应 #2068868
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04616038
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A solution of 1.41 g (10 mmole) of 3-cyclopentylpropionamide and 1.53 g (15 mmole) of 2-ketobutyric acid was stirred and refluxed under a small Dean-Stark trap. After 8 hrs the solution was cooled, resulting in heavy crystallization. The solid was collected on a filter and washed with toluene and CH2Cl2. Yeld of white crystals=1.44 g, mp 180.5°-182° (prelim. softening). The material was recrystallized from methyl ethyl ketone. Yield of white needles=0.63 g (28%), mp 184°-185° (slight prelim. softening). Tlc (4:1 toluene-AcOH) now showed a single spot, and NMR indicated essentially pure Z-isomer. refluxed under a small Dean-Stark trap After 8 hrs the solution was cooled resulting in heavy crystallization The solid was collected on a filter washed with toluene and CH2Cl2 The material was recrystallized from methyl ethyl ketone
来源 ID: ord-badde93eedb0497ab1ea3c933fd66cf8