反应详情

Thionyl chloride (2.55 mL, 35 mmol) was added dropwise to absolute ethanol (100 mL) under a N2 atmosphere. The resulting solution was stirred at room temperature for 10 min then 4-amino-1-cyclohexanecarboxylic acid (4.29 g, 30 mmol, cis, trans mixture) was added as a solid. The resulting solution was stirred at room temperature overnight. The solvent was removed in vacuo, the residue dissolved in ethanol (25 mL) and this solution was slowly added to a flask containing rapidly stirred ether (700 mL). The precipitate that formed was collected by filtration and dried in vacuo to give 5.75 g, 92% as a white solid. MS (ion spray) 172 (M+1).

1. stirringThe resulting solution was stirred at room temperature overnight
2. customThe solvent was removed in vacuo
3. dissolutionthe residue dissolved in ethanol (25 mL)
4. additionthis solution was slowly added to a flask
5. additioncontaining rapidly stirred ether (700 mL)
6. customThe precipitate that formed
7. filtrationwas collected by filtration
8. customdried in vacuo
9. customto give 5.75 g, 92% as a white solid