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Hexamethylenetetramine → HCID 19858062, Verbindung

HRID 2073387
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2073387
[CH3:1][C:2]1([CH3:17])[C:6](=[O:7])[O:5][C:4]2[CH:8]=[CH:9][C:10]3[C:15]([C:3]1=2)=[CH:14][C:13]([CH3:16])=[CH:12][CH:11]=3.FC(F)(F)[C:20](O)=[O:21].C1N2CN3CN(C2)CN1C3>>[CH:20]([C:12]1[CH:11]=[C:10]2[C:15](=[CH:14][C:13]=1[CH3:16])[C:3]1[C:2]([CH3:17])([CH3:1])[C:6](=[O:7])[O:5][C:4]=1[CH:8]=[CH:9]2)=[O:21]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 3

HCID 4101HexamethylenetetramineHCID 6422Trifluoroacetic acidHCID 19858068HCID 19858068, Verbindung

Produkt 1

HCID 19858062HCID 19858062, Verbindung

Versuchsvorschrift

A mixture of 1,1,8-trimethyl-2-(1H)-naphtho[2,1-b]furanone (3.85)g, trifluoracetic acid (25 ml) and hexamine (3.5 g) was stirred under reflux for 18 h. The bulk of the trifluoroacetic acid was evaporated under reduced pressure and the residue was treated with water and heated at 90° for 10 minutes. The mixture was neutralised with potassium hydrogen carbonate and extracted twice with chloroform. The combined extracts were dried and evaporated to dryness, and the residue was recrystallised from ethyl acetate to give 7-formyl-1,1,8-trimethyl-2(1H)-naphtho[2,1-b]furanone (2.2 g), m.p. 193°-195° C.

Aufarbeitung

  1. temperatureunder reflux for 18 h
  2. customThe bulk of the trifluoroacetic acid was evaporated under reduced pressure
  3. additionthe residue was treated with water
  4. temperatureheated at 90° for 10 minutes
  5. extractionextracted twice with chloroform
  6. customThe combined extracts were dried
  7. customevaporated to dryness
  8. customthe residue was recrystallised from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-37837a46ffaf41399e01530dd358d1aa
Quelldatensatz
uspto-grants-1990_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04916148

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