Dimethylformamide → (S)-1-((3-(1-(2,2-Difluoro-2-(1-hydroxy-3,3,5,5-tetramethylcyclohexyl)acetyl)pyrrolidin-2-yl)isoxazol-5-yl)methyl)pyridin-2(1H)-one
Reaktionsgleichung
CN(C=O)C.CS(O[CH2:11][C:12]1[O:16][N:15]=[C:14]([C@@H:17]2[CH2:21][CH2:20][CH2:19][N:18]2[C:22](=[O:37])[C:23]([F:36])([F:35])[C:24]2([OH:34])[CH2:29][C:28]([CH3:31])([CH3:30])[CH2:27][C:26]([CH3:33])([CH3:32])[CH2:25]2)[CH:13]=1)(=O)=O.[N:38]1[CH:43]=[CH:42][CH:41]=[CH:40][C:39]=1[OH:44].C([O-])([O-])=O.[K+].[K+]>CS(C)=O>[F:36][C:23]([F:35])([C:24]1([OH:34])[CH2:25][C:26]([CH3:32])([CH3:33])[CH2:27][C:28]([CH3:31])([CH3:30])[CH2:29]1)[C:22]([N:18]1[CH2:19][CH2:20][CH2:21][C@H:17]1[C:14]1[CH:13]=[C:12]([CH2:11][N:38]2[CH:43]=[CH:42][CH:41]=[CH:40][C:39]2=[O:44])[O:16][N:15]=1)=[O:37]Komponenten
6
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 50 °C
Versuchsvorschrift
To a DMF (1.0 mL) solution of the compound (30 mg) obtained in Example 3-(5) and pyridin-2-ol (12 mg), K2CO3 (35 mg) was added and the mixture was stirred at 50° C. for an hour. To the reaction mixture, DMSO (1.0 ml) was added and after filtering off the insoluble matter, the filtrate was purified by reverse-phase preparative HPLC to give Compound 54 (2.0 mg, colorless oil) and Compound 60 (16.0 mg, colorless oil.)
Aufarbeitung
- filtrationafter filtering off the insoluble matter
- customthe filtrate was purified by reverse-phase preparative HPLC
Quellen und Nachweise
- ORD-Eintrag
- ord-aa0c01ea92134f53992c520365560fa2
- Quelldatensatz
- uspto-grants-2015_11
- Patentnummer
- US09181229B2
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