Sodium Succinate → HCID 53682371, Verbindung

HRID 1578576

Reaktionsgleichung

Reaktionsgleichung von HRID 1578576
[C:1]([O-:8])(=[O:7])[CH2:2][CH2:3][C:4]([O-:6])=[O:5].[Na+].[Na+].[C:11]([N:15]=[N:16][C:17](Cl)([CH2:19][CH:20]([CH3:22])[CH3:21])[CH3:18])([CH3:14])([CH3:13])[CH3:12]>CN(C)C=O>[C:1]([O:8][C:17]([N:16]=[N:15][C:11]([CH3:14])([CH3:13])[CH3:12])([CH3:18])[CH2:19][CH:20]([CH3:21])[CH3:22])(=[O:7])[CH2:2][CH2:3][C:4]([O:6][C:17]([N:16]=[N:15][C:11]([CH3:14])([CH3:13])[CH3:12])([CH3:18])[CH2:19][CH:20]([CH3:22])[CH3:21])=[O:5]

Komponenten

4

Edukt 2

HCID 9020Sodium SuccinateHCID 23344796(E)-1-tert-Butyl-2-(2-chloro-4-methylpentan-2-yl)diazene

Produkt 1

HCID 53682371HCID 53682371, VerbindungAusbeute 60 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a slurry of 5.97 grams (.0221 moles) of sodium succinate in 75 mls. of dimethylformamide in a 200 beaker, warmed to 35°C in a water bath, was added 9.0 grams (.0442 moles) of 2-t-butylazo-2-chloro-4-methylpentane dropwise. After the addition was complete, the reaction was stirred for 3 hours at room temperature, poured into 200 ml. of cold water and extracted with pentane. The pentane solution was washed with water, dried over anhydrous Na2SO4, filtered, stirred over alumina, filtered and the pentane evaporated to leave 6.0 grams (60% yield) of a light yellow liquid. The crude product was purified by column chromatography using pentane as eluent. The infrared spectrum of the purified product was in agreement with the structure of the desired product.

Aufarbeitung

  1. additionAfter the addition
  2. additionpoured into 200 ml
  3. extractionof cold water and extracted with pentane
  4. washThe pentane solution was washed with water
  5. dry with materialdried over anhydrous Na2SO4
  6. filtrationfiltered
  7. stirringstirred over alumina
  8. filtrationfiltered
  9. customthe pentane evaporated

Quellen und Nachweise

ORD-Eintrag
ord-a51a7cee7c564a30aeec9185cee663d7
Quelldatensatz
uspto-grants-1976_02
Patentnummer
US03937761

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