反应 #1135043
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05668161
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of 4-phenylbutyramide (0.373 g, 2.28 mmol) in toluene (15 mL) was added Lawesson's reagent (0.461 g, 1.14 mmol). The reaction was refluxed overnight, cooled to room temperature and concentrated yielding an orange oil. Flash chromatography of this oil (1:1 hexane:methylene chloride with 1% acetic acid) yielded 4-phenylthiobutyramide (0.184 g) as a white solid: 1HNMR (DMSO d6 ) 400 mHz 9.33 (s, 1 H), 9.13 (s, 1 H), 7.29-7.23 (m, 2 H), 7.20-7.15 (m, 3 H), 2.56 (t, J=7.58 Hz, 2 H), 2.50-2.42 (m, 2 H), 2.00-1.85 (m, 2 H). The reaction was refluxed overnight concentrated yielding an orange oil
来源 ID: ord-e3ca98cc7da242a19e85566293cd2f8e