Piperidine → HCID 67005741、化合物
反応式
C1C2C(COC([N:18]3[CH2:23][CH2:22][N:21]([C:24](=[O:60])[C@@H:25]([N:33]([CH2:48][C:49]4[CH:54]=[CH:53][C:52]([CH2:55][CH2:56][CH2:57][CH2:58][CH3:59])=[CH:51][CH:50]=4)[C:34](=[O:47])[CH:35]=[CH:36][C:37]4[CH:42]=[CH:41][C:40]([C:43]([F:46])([F:45])[F:44])=[CH:39][CH:38]=4)[CH2:26][C:27]4[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=4)[CH2:20][CH2:19]3)=O)C3C(=CC=CC=3)C=2C=CC=1.N1CCCCC1.CCOC(C)=O>CN(C=O)C>[CH2:26]([C@H:25]([N:33]([CH2:48][C:49]1[CH:50]=[CH:51][C:52]([CH2:55][CH2:56][CH2:57][CH2:58][CH3:59])=[CH:53][CH:54]=1)[C:34](=[O:47])[CH:35]=[CH:36][C:37]1[CH:42]=[CH:41][C:40]([C:43]([F:46])([F:45])[F:44])=[CH:39][CH:38]=1)[C:24](=[O:60])[N:21]1[CH2:20][CH2:19][NH:18][CH2:23][CH2:22]1)[C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1参加物
5
実験手順
4-(2-{(4-pentyl-benzyl)-[3-(4-trifluoromethyl-phenyl)-acryloyl]-amino}-(S)-3-phenyl-propionyl)-piperazine-1-carboxylic acid 9H-fluoren-9-ylmethyl ester (1.75 g, 2.15 mmol) was dissolved in DMF (47.5 mL) and piperidine (2.5 mL) was added. Stirring was continued at rt for 30 min. EtOAc (150 mL) was added and the mixture was washed with water (2×150 mL). The organic layer was dried over magnesium sulfate, filtered and concentrated in vacuo. The residue was purified by column chromatography (silicagel, MeOH/DCM=1/99) to give 1.05 g (82.5%) of N—((S)-1-Benzyl-2-oxo-2-piperazin-1-yl-ethyl)-N-(4-pentyl-benzyl)-3-(4-trifluoromethyl-phenyl)-acrylamide. LC-MS: tR=0.97 min; [M+H]+=592.19.