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Sodium Chloride → HCID 22877878, Verbindung

HRID 1488849
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1488849
[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].C([NH:41][C@H:42]([C:44]([NH2:46])=[O:45])[CH3:43])(OCC1C2C(=CC=CC=2)C2C1=CC=CC=2)=O.[OH-].[Na+].[Cl-].[Na+]>CO>[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].[NH2:41][C@H:42]([C:44]([NH2:46])=[O:45])[CH3:43]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 5234Sodium ChlorideHCID 14798Sodium HydroxideHCID 22877914HCID 22877914, Verbindung

Produkt 1

HCID 22877878HCID 22877878, VerbindungAusbeute 87,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

One gram (1.6 mmols) of (Z)-1-(3-amino-4-methoxyphenyl)-2-(3,4,5-trimethoxyphenyl)-ethene-Fmoc-L-alanineamide was dissolved in 10 ml of methanol, and 0.9 ml (1.76 mmols) of an aqueous solution of 2-N sodium hydroxide were added thereto. The mixture was stirred for 3 hours. A saturated aqueous solution of sodium chloride 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 using a silica-gel plate (mixture of 5-% by volume methanol and dichloromethane) to produce 543 mg of the final compound in a yield of 87.9%.

Aufarbeitung

  1. extractionthe resulting mixture was extracted three times with dichloromethane
  2. dry with materialThe extract was dried over anhydrous sodium sulfate
  3. concentrationconcentrated to dryness under reduced pressure
  4. customThe product was purified
  5. additiona silica-gel plate (mixture of 5-% by volume methanol and dichloromethane)

Quellen und Nachweise

ORD-Eintrag
ord-548e0c024d0442089c014ce5294f8304
Quelldatensatz
uspto-grants-1997_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05674906

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