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Acetic Anhydride → HCID 178488951, Verbindung

HRID 235960
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 235960
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[NH:10][C:11]([N+:15]([O-])=O)=[C:12]([CH3:14])[N:13]=2)=[CH:5][CH:4]=1.[C:18](OC(=O)C)(=[O:20])[CH3:19].[H][H]>CC(O)=O.[Pt]>[C:18]([NH:15][C:11]1[NH:10][C:9]([C:6]2[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)=[N:13][C:12]=1[CH3:14])(=[O:20])[CH3:19]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 7918Acetic AnhydrideHCID 135671327HCID 135671327, VerbindungHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 178488951HCID 178488951, VerbindungAusbeute 84 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23939PlatinumKatalysator
HCID 176
Acetic Acid
Lösungsmittel

Versuchsvorschrift

A solution of 41 (3.5 g, 0.015 mole) dissolved in glacial HOAc (35 ml)--acetic anhydride (105 ml) was hydrogenated at 50 psi over 5% platinum on charcoal catalyst (0.75 g) until uptake of hydrogen was complete. Catalyst was filtered off and the filtrate was evaporated to dryness under reduced pressure. The residue was dissolved in H2O (50 ml) and heated on a steam bath for 1 hour. The cooled solution was washed with ether (4×10 ml) and then evaporated to dryness in vacuo. Recrystallization of the residue from CHCl3 gave 3.07 g (84%) of 42 in two crops; m.p. 202°-204° C.

Aufarbeitung

  1. filtrationCatalyst was filtered off
  2. customthe filtrate was evaporated to dryness under reduced pressure
  3. dissolutionThe residue was dissolved in H2O (50 ml)
  4. temperatureheated on a steam bath for 1 hour
  5. washThe cooled solution was washed with ether (4×10 ml)
  6. customevaporated to dryness in vacuo
  7. customRecrystallization of the residue from CHCl3

Quellen und Nachweise

ORD-Eintrag
ord-94915cc999144073835cdb7647951dec
Quelldatensatz
uspto-grants-1987_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04642311

Notizen zur Reaktion

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