2,2,2-Trifluoroethanol → HCID 67938850, Verbindung

HRID 622705Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 622705
[F:1][C:2]([F:6])([F:5])[CH2:3][OH:4].[H-].[Na+].[Na].Br[C:11]1[CH:16]=[CH:15][C:14]([CH2:17][N:18]2[CH2:22][CH2:21][NH:20][C:19]2=[CH:23][N+:24]([O-:26])=[O:25])=[CH:13][N:12]=1>C1(C)C=CC=CC=1>[F:1][C:2]([F:6])([F:5])[CH2:3][O:4][C:11]1[CH:16]=[CH:15][C:14]([CH2:17][N:18]2[CH2:22][CH2:21][NH:20][C:19]2=[CH:23][N+:24]([O-:26])=[O:25])=[CH:13][N:12]=1

Komponenten

6

Edukt 4

HCID 64092,2,2-Trifluoroethanol2×HCID 24758Sodium hydrideHCID 5360545SodiumHCID 85528837HCID 85528837, Verbindung

Produkt 1

HCID 67938850HCID 67938850, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

2,2,2-Trifluoroethanol (3.6 g) was dissolved in toluene (20 ml), and sodium hydride (0.7 g) was added to prepare a sodium salt of 2,2,2-trifluoroethanol. Then, 3 g of 1-(2-bromo-5-pyridylmethyl)-2-(nitromethylene)imidazolidine (the known compound described in Japanese Patent Application No. 132,943/1984) was added, and the mixture was heated at 80° C. for 8 hours. Toluene was distilled off under reduced pressure, and the residue was poured into 20 ml of ice water and then neutralized. The aqueous solution was extracted with dichloromethane, and the extract was purified by silica gel column chromatography to give 1-[2-(2,2,2-trifluoroethoxy)-5-pyridylmethyl]-2-(nitromethylene)-imidazolidine. mp. 132°-135° C.

Aufarbeitung

  1. addition132,943/1984) was added
  2. distillationToluene was distilled off under reduced pressure
  3. additionthe residue was poured into 20 ml of ice water
  4. extractionThe aqueous solution was extracted with dichloromethane
  5. customthe extract was purified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-f16100821cc943d5b3100d9fffe02296
Quelldatensatz
uspto-grants-1988_09
Patentnummer
US04772620

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