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Dimethylformamide → HCID 89875881, Verbindung

HRID 1048634
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1048634
[CH3:1][C:2]1[C:7]([O:8][CH2:9][CH3:10])=[CH:6][CH:5]=[CH:4][C:3]=1[N:11]1[C:15](=[O:16])[NH:14][N:13]=[N:12]1.[C:17](=O)([O-])[O-].[K+].[K+].CN(C)C=O.S(OC)(OC)(=O)=O>O>[CH3:1][C:2]1[C:7]([O:8][CH2:9][CH3:10])=[CH:6][CH:5]=[CH:4][C:3]=1[N:11]1[C:15](=[O:16])[N:14]([CH3:17])[N:13]=[N:12]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 6228DimethylformamideHCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 136646183HCID 136646183, Verbindung

Produkt 1

HCID 89875881HCID 89875881, VerbindungAusbeute 92,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962
Water
Lösungsmittel

Versuchsvorschrift

Under ice-cooling, to a mixture of 1-(2-methyl-3-ethoxyphenyl)-1,4-dihydrotetrazole-5-one 39.0 g, potassium carbonate 36.7 g and N,N-dimethylformamide 400 mL was added dimethyl sulfate 44.7 g and the resulting mixtures were raised to room temperature and were stirred for seven hours. Thereto was added water and the mixtures were extracted with ethyl acetate and the organic layers were washed with water and saturated saline, and were dried over anhydrous magnesium sulfate and were then concentrated under reduced pressure. The resulting residues were subjected to a silica gel column chromatography to give 1-(2-methyl-3-ethoxyphenyl)-4-methyl-1,4-dihydrotetrazole-5-one 38.2 g.

Aufarbeitung

  1. extractionthe mixtures were extracted with ethyl acetate
  2. washthe organic layers were washed with water and saturated saline
  3. dry with materialwere dried over anhydrous magnesium sulfate
  4. concentrationwere then concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-8d0888b8740646e186ceb30047fdf103
Quelldatensatz
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09380782B2

Notizen zur Reaktion

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