Sodium hydride → Oxadixyl

HRID 67905

Reaktionsgleichung

Reaktionsgleichung von HRID 67905
[CH3:1][O:2][CH2:3][C:4]([N:6]([C:14]1[C:19]([CH3:20])=[CH:18][CH:17]=[CH:16][C:15]=1[CH3:21])[NH:7][C:8]([O:10][CH2:11][CH2:12]Cl)=[O:9])=[O:5].[H-].[Na+]>C1(C)C=CC=CC=1>[CH3:1][O:2][CH2:3][C:4]([N:6]([C:14]1[C:19]([CH3:20])=[CH:18][CH:17]=[CH:16][C:15]=1[CH3:21])[N:7]1[CH2:12][CH2:11][O:10][C:8]1=[O:9])=[O:5]

Komponenten

4

Edukt 2

HCID 24758Sodium hydrideHCID 204544942-Chloroethyl 2-(methoxyacetyl)-2-(2,6-dimethylphenyl)-hydrazinecarboxylate

Produkt 1

HCID 53735Oxadixyl

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

11.8 g (0.0375 mol) 2-Chloroethyl 2-(methoxyacetyl)-2-(2,6-dimethylphenyl)-hydrazinecarboxylate are added portion-wise to a suspension of 2.0 g sodium hydride (in form of about 55% by weight in mineral oil) in 100 ml absolute toluene at room temperature under a blanket of nitrogen. The reaction temperature rises gradually during this addition up to 40°. After the addition is complete the mixture is stirred during 30 minutes without cooling and afterwards cooled to 10°. The unreacted sodium hydride is then destroyed with ethanol, the obtained solution washed with water dried with MgSO4 and the solvent removed in vacuo to give the end title compound which is recrystallised from ethanol to yield the title compound as colourless crystals. m.p. 103°-104°.

Aufarbeitung

  1. additionThe reaction temperature rises gradually during this addition up to 40°
  2. additionAfter the addition
  3. temperaturewithout cooling
  4. temperatureafterwards cooled to 10°
  5. customThe unreacted sodium hydride is then destroyed with ethanol
  6. washthe obtained solution washed with water
  7. dry with materialdried with MgSO4
  8. customthe solvent removed in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-fffd76d46a214db79031677a4bdceb18
Quelldatensatz
uspto-grants-1982_08
Patentnummer
US04347253

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