Triethylamine → HCID 10899796、化合物

反応式

[F:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH2:4]Cl.O.Cl.[NH:12]1[CH2:17][CH2:16][C:15](=[O:18])[CH2:14][CH2:13]1.C(N(CC)CC)C>ClCCl>[F:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH2:4][N:12]1[CH2:17][CH2:16][C:15](=[O:18])[CH2:14][CH2:13]1

参加物

実験手順

64.00 g (0.443 mol) of o-fluorobenzylchloride was weighed, to which 250 mL of dichloromethane was added. 62.40 g (0.406 mol) of 4-piperidone hydrochloride monohydrate was added under stirring, and then 91.00 g (0.899 mol) of triethylamine was added dropwise under cold water cooling and stirring. The reaction was stirred at room temperature for 4.5 h, and then stirred under reflux and reacted overnight. On the next day, the reaction was cooled, filtered to remove solid, washed in sequence with dichloromethane and ethyl ether, combined, washed with water and dried, and the solvent was recovered to obtain 68.95 g crude product (82.00%), which was used directly in the next reaction.