Reaktionsgleichung
C(O[C:6]([NH:8][CH2:9][CH2:10][O:11][C:12]1[CH:17]=[C:16]([C:18]#[N:19])[CH:15]=[CH:14][C:13]=1[CH:20]=[CH:21][C:22]([O:24][CH2:25][CH3:26])=[O:23])=[O:7])(C)(C)C.Cl.[N:28]1[CH:33]=[CH:32][C:31]([N:34]2[CH2:39][CH2:38][CH:37](C(O)=O)[CH2:36][CH2:35]2)=[CH:30][CH:29]=1.F[P-](F)(F)(F)(F)F.Br[P+](N1CCCC1)(N1CCCC1)N1CCCC1.C(N(CC)CC)C>Cl.O1CCOCC1>[C:18]([C:16]1[CH:15]=[CH:14][C:13]([CH:20]=[CH:21][C:22]([O:24][CH2:25][CH3:26])=[O:23])=[C:12]([O:11][CH2:10][CH2:9][NH:8][C:6]([CH:37]2[CH2:36][CH2:35][N:34]([C:31]3[CH:32]=[CH:33][N:28]=[CH:29][CH:30]=3)[CH2:39][CH2:38]2)=[O:7])[CH:17]=1)#[N:19]Komponenten
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Versuchsvorschrift
3.0 g (8.33 mmol) of ethyl 3-[2-(2-(t-butoxycarbonylamino)ethoxy)-4-cyanophenyl]acrylate was dissolved in a mixture of 20 ml of 4 N solution of hydrogen chloride in dioxane and 10 ml of dioxane. The obtained solution was stirred at room temperature for 4 hours. The solvent was evaporated and the residue was dissolved in 50 ml of DMF. 2.22 g (9.17 mmol) of 1-(4-pyridyl)-4-piperidinecarboxyic acid hydrochloride, 4.27 g (9.17 mmol) of bromotripyrrolidinophosphonium hexafluorophosphate and 3.48 ml (25.0 mmol) of triethylamine were added to the obtained solution, and they were stirred at room temperature for 3 days. The solvent was evaporated, and the obtained crude product was purified by the silica gel column chromatography to obtain the title compound.
Aufarbeitung
- customThe solvent was evaporated
- dissolutionthe residue was dissolved in 50 ml of DMF
- stirringwere stirred at room temperature for 3 days
- customThe solvent was evaporated
- customthe obtained crude product
- customwas purified by the silica gel column chromatography
Quellen und Nachweise
- ORD-Eintrag
- ord-f4db89e8ac694c4d9a71466786e1719b
- Quelldatensatz
- uspto-grants-2002_06
- Patentnummer
- US06410538B2
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