Methanol → 3,5-Dimethyl-2-hydroxymethyl-4-(2,2,3,3,3-pentafluoropropoxy)pyridine

HRID 622158Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 622158
[CH3:1][C:2]1[CH:3]=[N+:4]([O-])[CH:5]=[C:6]([CH3:17])[C:7]=1[O:8][CH2:9][C:10]([F:16])([F:15])[C:11]([F:14])([F:13])[F:12].S(OC)([O:22][CH3:23])(=O)=O.CO.S(OOS([O-])(=O)=O)([O-])(=O)=O.[NH4+].[NH4+]>O>[CH3:1][C:2]1[C:3]([CH2:23][OH:22])=[N:4][CH:5]=[C:6]([CH3:17])[C:7]=1[O:8][CH2:9][C:10]([F:16])([F:15])[C:11]([F:14])([F:13])[F:12]

Komponenten

6

Edukt 4

HCID 887Methanol2×HCID 6497Dimethyl SulfateHCID 62648Ammonium PersulfateHCID 136548073,5-Dimethyl-4-(2,2,3,3,3-pentafluoropropoxy)pyridine-1-oxide

Produkt 1

HCID 149020163,5-Dimethyl-2-hydroxymethyl-4-(2,2,3,3,3-pentafluoropropoxy)pyridine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

A mixture of 3,5-dimethyl-4-(2,2,3,3,3-pentafluoropropoxy)pyridine-1-oxide (2.5 g) and dimethyl sulfate (1 ml) was heated at 120° C. for 30 minutes and methanol (12.5 ml) was added, after which a solution of ammonium persulfate (4.3 g) in water (20 ml)-methanol (10 ml) was added dropwise at 80° C. over a period of 30 minutes and the mixture was stirred for 30 minutes. After concentration, ice was added and the mixture was neutralized with sodium carbonate, and then was extracted with chloroform. After drying the extract over sodium sulfate, the solvent was evaporated to give 2.2 g of 3,5-dimethyl-2-hydroxymethyl-4-(2,2,3,3,3pentafluoropropoxy)pyridine as oil.

Aufarbeitung

  1. concentrationAfter concentration, ice
  2. additionwas added
  3. extractionwas extracted with chloroform
  4. customAfter drying the
  5. extractionextract over sodium sulfate
  6. customthe solvent was evaporated

Quellen und Nachweise

ORD-Eintrag
ord-2470191b9cc84d31a7bb1d8528010a67
Quelldatensatz
uspto-grants-1988_09
Patentnummer
US04769456

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