Azobisisobutyronitrile → HCID 178459095, Verbindung

HRID 1972299

Reaktionsgleichung

Reaktionsgleichung von HRID 1972299
CC(N=NC(C#N)(C)C)(C#N)C.C[CH2:14][C:15]([CH2:20][O:21][CH2:22][CH:23]=[CH2:24])(CO)CO.[C:25]([OH:30])(=[S:29])[CH:26]([CH3:28])[OH:27]>CO.C1(C)C=CC=CC=1.CCCCCC>[CH2:20]([O:21][CH2:22][CH:23]=[CH2:24])[CH:15]=[CH2:14].[C:25]([OH:30])(=[S:29])[CH:26]([CH3:28])[OH:27]

Komponenten

7

Edukt 3

HCID 6547AzobisisobutyronitrileHCID 12683Trimethylolpropane monoallyl etherHCID 178473673HCID 178473673, Verbindung

Produkt 1

HCID 178459095HCID 178459095, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 887MethanolLösungsmittelHCID 1140TolueneLösungsmittelHCID 8058HexaneLösungsmittel

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

AIBN (1.5 g) was dissolved in trimethylolpropane monoallyl ether (497 g, 2.86 mol). This solution was slowly added, under nitrogen with stirring, to thiolactic acid (300 g, 2.83 mol) at such a rate that the temperature of the exothermal reaction was kept at 80° C. When the addition was completed, the temperature was raised to 90° C. and kept at 90° C. for 1 h. The product had 1H-NMR (CDCl3): δ 1.11 (t, 3H, CH3CH2), 1.53 (q, 2H, CH3CH2), 2.00-2.20 (m, 2H, CH2CH2CH2), 2.98-3.06 (m, 2H, 3.65-4.02 (m, 9H); and is soluble in methanol and toluene, not soluble in hexane.

Aufarbeitung

  1. additionThis solution was slowly added, under nitrogen
  2. customthat the temperature of the exothermal reaction
  3. customwas kept at 80° C
  4. additionWhen the addition

Quellen und Nachweise

ORD-Eintrag
ord-641a1f01701d42dc9ace8d49418ea828
Quelldatensatz
uspto-grants-2013_04
Patentnummer
US08431748B2

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