Water → HCID 21412720, Verbindung

HRID 2071862Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2071862
C(=O)([O-])O[O:3][O:4][C:5]([CH3:8])([CH3:7])[CH3:6].[K+].CN(C)[CH:14]=[O:15].[C:17]([N:21]=[N:22][C:23](Cl)([CH2:25][CH3:26])[CH3:24])([CH3:20])([CH3:19])[CH3:18].[OH2:28]>CCCCC>[C:17]([N:21]=[N:22][C:23]([O:28][C:14]([O:3][O:4][C:5]([CH3:6])([CH3:7])[CH3:8])=[O:15])([CH2:25][CH3:26])[CH3:24])([CH3:20])([CH3:19])[CH3:18]

Komponenten

6

Edukt 4

HCID 962WaterHCID 6228DimethylformamideHCID 10773630Diazene, (1-chloro-1-methylpropyl)(1,1-dimethylethyl)-HCID 23708493HCID 23708493, Verbindung

Produkt 1

HCID 21412720HCID 21412720, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8003PentaneLösungsmittel

Versuchsvorschrift

To a stirred slurry of 18.9 grams (0.11 mole) potassium t-butylperoxy carbonate in 80 ml. of N,N-dimethylformamide in a 250 ml round bottom flask was slowly added 17.66 grams (0.1 mole)2-t-butylazo-2-chlorobutane. After the addition was complete the reaction was stirred for 5 hours at room temperature and poured into 350 ml water. The product was taken up in 100 ml pentane and the pentane solution washed with 5% HCl, water and saturated sodium bicarbonate solution. The pentane solution was dried over anhydrous sodium sulfate, filtered and the pentane evaporated under reduced pressure. The residue weighed 22.9 grams (83% yield) and its infrared spectrum was in agreement with the structure of 2-t-butylazo-2-(t-butyl-peroxycarbonyloxy)butane (strong carbonyl band at 1750 cm31 1).

Aufarbeitung

  1. additionAfter the addition
  2. washthe pentane solution washed with 5% HCl, water and saturated sodium bicarbonate solution
  3. dry with materialThe pentane solution was dried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. customthe pentane evaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-15ab07b800e24577944100901183f136
Quelldatensatz
uspto-grants-1977_09
Patentnummer
US04048423

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