Dichloromethane → HCID 68428933, Verbindung

HRID 2240287Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2240287
ClCCl.[CH3:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([NH:12][NH2:13])=[CH:8][CH:7]=1.C(N(CC)CC)C.[C:21](Cl)(=[O:26])[C:22]([CH3:25])([CH3:24])[CH3:23]>O>[CH3:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([NH:12][NH:13][C:21](=[O:26])[C:22]([CH3:25])([CH3:24])[CH3:23])=[CH:8][CH:7]=1

Komponenten

6

Edukt 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 62493Pivaloyl chlorideHCID 77023(4-Methoxyphenyl)hydrazine

Produkt 1

HCID 68428933HCID 68428933, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To a mixture of 50 ml of dichloromethane and 2.76 g of free 4-methoxyphenyl-hydrazine there are added first 2.2 g of triethylamine and then, dropwise, at a temperature of from 0° to 5°, 2.65 g of pivaloyl chloride. The reaction mixture is stirred for 12 hours at room temperature and then discharged into water. The aqueous mixture is extracted with dichloromethane, the extract is concentrated and the residue is recrystallised from toluene/pentane, yielding N-(4-methoxyphenyl)-N′-pivaloyl-hydrazine which melts at from 126° to 127°.

Aufarbeitung

  1. extractionThe aqueous mixture is extracted with dichloromethane
  2. concentrationthe extract is concentrated
  3. customthe residue is recrystallised from toluene/pentane

Quellen und Nachweise

ORD-Eintrag
ord-2fabd1ebcf9a44c6b47c6be027082d0f
Quelldatensatz
uspto-grants-2010_05
Patentnummer
US07723362B2

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