Pyridine → 1,2-butandiol Dibenzoate

HRID 132707

Reaktionsgleichung

Reaktionsgleichung von HRID 132707
[CH2:1]([OH:6])[CH:2]([OH:5])[CH2:3][CH3:4].[C:7](Cl)(=[O:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.N1C=C[CH:19]=[CH:18][CH:17]=1.[O:22]1[CH2:26][CH2:25][CH2:24][CH2:23]1>O>[C:7]([O:6][CH2:1][CH:2]([O:5][C:26](=[O:22])[C:25]1[CH:19]=[CH:18][CH:17]=[CH:23][CH:24]=1)[CH2:3][CH3:4])(=[O:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

Komponenten

6

Edukt 4

HCID 1049PyridineHCID 7412Benzoyl chlorideHCID 8028TetrahydrofuranHCID 114291,2-Butanediol

Produkt 1

HCID 231259061,2-butandiol Dibenzoate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To the reactor were added 1,2-butylene-glycol (2.5 g), benzoyl chloride (7.8 g), pyridine (8.8 g) and tetrahydrofuran (70 ml). The reactants was mixed and heated refluxing for 4 hours, then cooled to room temperature. Water was added to the reaction system until the inorganic phase was transparent. Organic phase was separated. Inorganic phase was extracted with ethyl ether. The combined organic phase was washed with water, dried over anhydrous sodium sulfate. After concentrated, 3.95 g product was separated. 1H-NMR: δ (ppm)1.0-1.1 (3H), 1.7-1.9(2H), 4.4-4.6(2H), 5.4-5.5(1H) and 7.4-8.2(10H).

Aufarbeitung

  1. additionThe reactants was mixed
  2. temperatureheated
  3. temperaturerefluxing for 4 hours
  4. customOrganic phase was separated
  5. extractionInorganic phase was extracted with ethyl ether
  6. washThe combined organic phase was washed with water
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationAfter concentrated
  9. custom3.95 g product was separated

Quellen und Nachweise

ORD-Eintrag
ord-b78bc78a8a854a8a814d4a63cfdec3ef
Quelldatensatz
uspto-grants-2008_06
Patentnummer
US07388061B2

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