Sodium peroxide → HCID 20367916, Verbindung

HRID 616580

Reaktionsgleichung

Reaktionsgleichung von HRID 616580
[O-:1][O-:2].[Na+].[Na+].[C:5]([N:9]=[N:10][C:11]1(Cl)[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1)([CH3:8])([CH3:7])[CH3:6]>CO>[C:5]([N:9]=[N:10][C:11]1([O:1][O:2][C:11]2([N:10]=[N:9][C:5]([CH3:8])([CH3:7])[CH3:6])[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]2)[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1)([CH3:8])([CH3:7])[CH3:6]

Komponenten

4

Edukt 2

HCID 14803Sodium peroxideHCID 233447841-t-Butylazo-1-chlorocyclohexane

Produkt 1

HCID 20367916HCID 20367916, VerbindungAusbeute 100,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a solution of 0.78 grams (.01 moles) of sodium peroxide in 30 ml. of methanol, cooled to 10° C in a 50 ml. erlenmeyer flask immersed in a cold water bath was added 4.3 grams (.0213 moles) of 1-t-butylazo-1-chlorocyclo-hexane dropwise and with rapid stirring holding the temperature at 10°-15° C. After the addition was complete, the reaction was stirred for 1 hour at 5° C. It was then poured in 250 ml. of ice cold water and the product extracted with pentane. The pentane layer was separated, washed with saturated (NH4)2SO4, water, saturated NaHCO3, water, dried, filtered and the pentane evaporated under reduced pressure to give 3.67 grams (85% yield) of crude di[1-(t-butylazo)cyclohexyl] peroxide. The infrared spectrum indicated the product was contaminated to a small extent by 1-t-butylazo-1-methoxy-cyclohexane which resulted from the chloro compound reacting to a small extent with the methanol solvent.

Aufarbeitung

  1. customerlenmeyer flask immersed in a cold water bath
  2. customat 10°-15° C
  3. additionAfter the addition
  4. stirringthe reaction was stirred for 1 hour at 5° C
  5. additionIt was then poured in 250 ml
  6. extractionof ice cold water and the product extracted with pentane
  7. customThe pentane layer was separated
  8. washwashed with saturated (NH4)2SO4, water, saturated NaHCO3, water
  9. customdried
  10. filtrationfiltered
  11. customthe pentane evaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-4648701b3c0c48e7a5cd47961c5580c5
Quelldatensatz
uspto-grants-1978_02
Patentnummer
US04075199

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