1,1-Dimethylhydrazine → HCID 136166736, Verbindung

HRID 652792Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 652792
[C:1]([C:5]1[CH:6]=[C:7]([CH:16]=[C:17]([C:20]([CH3:23])([CH3:22])[CH3:21])[C:18]=1[OH:19])[C:8]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)=O)([CH3:4])([CH3:3])[CH3:2].[CH3:24][N:25]([CH3:27])[NH2:26].C1(C)C=CC(S(O)(=O)=O)=CC=1>O>[CH3:24][N:25]([CH3:27])[N:26]=[C:8]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[C:7]1[CH:6]=[C:5]([C:1]([CH3:4])([CH3:3])[CH3:2])[C:18]([OH:19])=[C:17]([C:20]([CH3:23])([CH3:22])[CH3:21])[CH:16]=1

Komponenten

5

Edukt 3

HCID 59761,1-DimethylhydrazineHCID 6101p-Toluenesulfonic acidHCID 1898376(3,5-Di-tert-butyl-4-hydroxyphenyl)(phenyl)methanone

Produkt 1

HCID 136166736HCID 136166736, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

One gram of 3,5-di-t-butyl-4-hydroxybenzophenone was added to 2 ml of 1,1-dimethylhydrazine, and the mixture was heated at 70° to 75° C. for 8 hours in the presence of 20 mg of p-toluenesulfonic acid in autoclave. After cooling, the reaction mixture was poured into water and extracted with diethyl ether. The ethereal layer was washed with water and dried. The ether was distilled, and the residue was chromatographed on a silica gel column, and recrystallized from diethyl ether to give 3,5-di-t-butyl-4-hydroxybenzophenone dimethylhydrazone as pale yellow needles.

Aufarbeitung

  1. temperatureAfter cooling
  2. extractionextracted with diethyl ether
  3. washThe ethereal layer was washed with water
  4. customdried
  5. distillationThe ether was distilled
  6. customthe residue was chromatographed on a silica gel column
  7. customrecrystallized from diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-54c54bad9082412b9192c9549d67a5bf
Quelldatensatz
uspto-grants-1987_06
Patentnummer
US04673692

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