Diisopropylethylamine → HCID 69034747, Verbindung
Reaktionsgleichung
[CH2:1]([O:3][C:4](=[O:19])[CH2:5][CH2:6][CH2:7][N:8]1[C:12]2[N:13]=[C:14]([CH3:18])[N:15]=[C:16](Cl)[C:11]=2[CH:10]=[CH:9]1)[CH3:2].[C:20]([O:24][C:25](=[O:40])[C@H:26]([CH2:38][SH:39])[NH:27][S:28]([C:31]1[CH:36]=[CH:35][C:34]([Br:37])=[CH:33][CH:32]=1)(=[O:30])=[O:29])([CH3:23])([CH3:22])[CH3:21].CCN(C(C)C)C(C)C>CN1C(=O)CCC1>[CH2:1]([O:3][C:4](=[O:19])[CH2:5][CH2:6][CH2:7][N:8]1[C:12]2[N:13]=[C:14]([CH3:18])[N:15]=[C:16]([S:39][CH2:38][C@H:26]([NH:27][S:28]([C:31]3[CH:36]=[CH:35][C:34]([Br:37])=[CH:33][CH:32]=3)(=[O:29])=[O:30])[C:25]([O:24][C:20]([CH3:22])([CH3:23])[CH3:21])=[O:40])[C:11]=2[CH:10]=[CH:9]1)[CH3:2]Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 100 °C
Versuchsvorschrift
279 mg of 4-(4-chloro-2-methyl-pyrrolo[2,3-d]pyrimidin-7-yl)-butyric acid ethyl ester (example 2a) and 655 mg of N-(4-bromobenzenesulfonyl)-(R)-cysteine-tert-butyl ester (example 6b) were dissolved in 2 ml of NMP and 0.68 ml of DIPEA were added. The reaction mixture was heated to 100° C. for 4 h. The mixture was diluted with 60 ml of EE and extracted with 10% citric acid, saturated NaCl solution and with water. The organic phase was dried over MgSO4 and the solvent was removed in vacuo. The crude product was chromatographed on silica gel eluting with EE/toluene (1:6). Yield: 108 mg.
Aufarbeitung
- additionThe mixture was diluted with 60 ml of EE
- extractionextracted with 10% citric acid, saturated NaCl solution and with water
- dry with materialThe organic phase was dried over MgSO4
- customthe solvent was removed in vacuo
- customThe crude product was chromatographed on silica gel eluting with EE/toluene (1:6)
Quellen und Nachweise
- ORD-Eintrag
- ord-774ca723c1db4ff2acb7aba3d033b0ee
- Quelldatensatz
- uspto-grants-2007_08
- Patentnummer
- US07259159B2
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