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Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphate → HCID 22877914, Verbindung

HRID 1488848
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1488848
[NH2:1][C:2]1[CH:3]=[C:4](/[CH:10]=[CH:11]\[C:12]2[CH:17]=[C:16]([O:18][CH3:19])[C:15]([O:20][CH3:21])=[C:14]([O:22][CH3:23])[CH:13]=2)[CH:5]=[CH:6][C:7]=1[O:8][CH3:9].[NH:24]([C:30]([O:32][CH2:33][CH:34]1[C:46]2[C:41](=[CH:42][CH:43]=[CH:44][CH:45]=2)[C:40]2[C:35]1=[CH:36][CH:37]=[CH:38][CH:39]=2)=[O:31])[C@H:25]([C:27](O)=[O:28])[CH3:26].C[N:48]([P+](ON1N=NC2C=CC=CC1=2)(N(C)C)N(C)C)C.F[P-](F)(F)(F)(F)F.C(=O)([O-])O.[Na+]>CN(C)C=O>[NH2:1][C:2]1[CH:3]=[C:4](/[CH:10]=[CH:11]\[C:12]2[CH:13]=[C:14]([O:22][CH3:23])[C:15]([O:20][CH3:21])=[C:16]([O:18][CH3:19])[CH:17]=2)[CH:5]=[CH:6][C:7]=1[O:8][CH3:9].[C:30]([NH:24][C@H:25]([C:27]([NH2:48])=[O:28])[CH3:26])([O:32][CH2:33][CH:34]1[C:35]2[C:40](=[CH:39][CH:38]=[CH:37][CH:36]=2)[C:41]2[C:46]1=[CH:45][CH:44]=[CH:43][CH:42]=2)=[O:31]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 516892Sodium BicarbonateHCID 6364642N-((9H-Fluoren-9-ylmethoxy)carbonyl)-L-alanineHCID 9796936AC-7739 free base

Produkt 1

HCID 22877914HCID 22877914, VerbindungAusbeute 41,5 %

Reagenzien, Katalysatoren, Lösungsmittel

1
HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

(Z)-1-(3-Amino-4-methoxyphenyl)-2-(3,4,5-trimethoxyphenyl)-ethene (2.2 g, 6.9 mmols), 2.7 g (8.3 mmols) of Fmoc-L-Ala and 12.1 g (27.6 mmols) of a BOP reagent were dissolved in 22 ml of N,N-dimethylformamide, and the mixture was heated at 60° C. for 4 hours. After the reaction mixture was cooled, a saturated aqueous solution of sodium hydrogencarbonate was added thereto, and the resulting mixture was extracted three times with dichloromethane. The extract was dried over anhydrous sodium sulfate, and concentrated to dryness under reduced pressure. The product was purified through silica-gel column chromatography (mixture of ethyl acetate and hexane at a ratio of 1:2) to produce 1.79 g of the final product in a yield of 41.4%.

Aufarbeitung

  1. temperatureAfter the reaction mixture was cooled
  2. extractionthe resulting mixture was extracted three times with dichloromethane
  3. dry with materialThe extract was dried over anhydrous sodium sulfate
  4. concentrationconcentrated to dryness under reduced pressure
  5. customThe product was purified through silica-gel column chromatography (
  6. additionmixture of ethyl acetate and hexane at a ratio of 1:2)

Quellen und Nachweise

ORD-Eintrag
ord-dd07457074c04c1b99d4ae14bde1cd3d
Quelldatensatz
uspto-grants-1997_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05674906

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