4-Methylmorpholine → HCID 131720134、化合物

反応式

[N:1]1([C:9]([O:11][CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[O:10])[CH2:8][CH2:7][CH2:6][C@H:2]1[C:3](Cl)=[O:4].Cl.[F:20][C:21]([F:33])([C:29]([F:32])([F:31])[F:30])[C:22]([CH:24]1[CH2:28][CH2:27][CH2:26][NH:25]1)=[O:23].CN1CCOCC1>C(Cl)Cl>[F:33][C:21]([F:20])([C:29]([F:30])([F:31])[F:32])[C:22]([CH:24]1[CH2:28][CH2:27][CH2:26][N:25]1[C:3]([CH:2]1[CH2:6][CH2:7][CH2:8][N:1]1[C:9]([O:11][CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)=[O:10])=[O:4])=[O:23]

参加物

実験手順

Methylene chloride (10 ml) was added to CBZ-L-Pro-Cl which was then reacted under argon with a suspension of 2-(2,2,3,3,3-pentafluoro-1-oxopropyl)pyrrolidine hydrochloride (compound from Example IC; 2.49 mmol) and N-methylmorpholine (0.54 ml; 4.98 mmol) dissolved in methylene chloride (7 ml). After 2.5 hours the reaction was concentrated and brought up in methylene chloride (1 ml) and the product purified by flash chromatography on silica gel column eluting with ethyl acetate/hexane (50:50). Product fractions were collected and concentrated to give the desired product (0.52 g) as a colorless oil.