反应详情

A solution of trans-4-trifluoromethylcyclohexanecarboxylic acid (0.5 g, 2.55 mmol) in thionyl chloride (3.70 mL, 51.0 mmol) was heated to 60° C. for 1 h, cooled to RT and concentrated to dryness. The material was co-evaporated with toluene (2×), dissolved in EtOAc (5 mL), treated with satd. NaHCO3 (5 mL) followed by NH4OH (˜13M, 0.588 mL, ˜7.65 mmol) and stirred at RT for 0.5 h. The layers were separated, the aqueous layer extracted with EtOAc (2×) and the combined organics were dried over Na2SO4 and concentrated to dryness to afford trans-4-(trifluoromethyl)cyclohexanecarboxamide (380 mg, 76%) as a white solid.

1. concentrationconcentrated to dryness
2. dissolutiondissolved in EtOAc (5 mL)
3. additiontreated with satd
4. customThe layers were separated
5. extractionthe aqueous layer extracted with EtOAc (2×)
6. dry with materialthe combined organics were dried over Na2SO4
7. concentrationconcentrated to dryness