1,4-Dioxane → 3-(3-Isocyanato-4-methoxyphenyl)-1-trifluoroacetyl-piperidine

HRID 1762122Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1762122
[NH2:1][C:2]1[CH:3]=[C:4]([CH:10]2[CH2:15][CH2:14][CH2:13][N:12]([C:16](=[O:21])[C:17]([F:20])([F:19])[F:18])[CH2:11]2)[CH:5]=[CH:6][C:7]=1[O:8][CH3:9].[O:22]1CCOC[CH2:23]1>ClC(OC(Cl)(Cl)Cl)=O>[N:1]([C:2]1[CH:3]=[C:4]([CH:10]2[CH2:15][CH2:14][CH2:13][N:12]([C:16](=[O:21])[C:17]([F:20])([F:18])[F:19])[CH2:11]2)[CH:5]=[CH:6][C:7]=1[O:8][CH3:9])=[C:23]=[O:22]

Komponenten

4

Edukt 2

HCID 312751,4-DioxaneHCID 137550743-(3-Amino-4-methoxyphenyl)-1-trifluoroacetyl piperidine

Produkt 1

HCID 200425593-(3-Isocyanato-4-methoxyphenyl)-1-trifluoroacetyl-piperidine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 10426DiphosgeneLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

6.04 g of 3-(3-amino-4-methoxyphenyl)-1-trifluoroacetyl piperidine in 120 ml of dioxane and 2.9 ml of trichloromethyl chloroformate were mixed together and stirred for 4 hours at 80° C. Then, the mixture was evaporated to dryness under reduced pressure. The residue was chromatographed on silica and eluted with a mixture of cyclohexane and ethyl acetate (7-3) to obtain 6.4 g of crude product which was used as is for the following step.

Aufarbeitung

  1. customThen, the mixture was evaporated to dryness under reduced pressure
  2. customThe residue was chromatographed on silica
  3. washeluted with a mixture of cyclohexane and ethyl acetate (7-3)

Quellen und Nachweise

ORD-Eintrag
ord-95a8c1cf24384903b231f4af39031dbe
Quelldatensatz
uspto-grants-1989_05
Patentnummer
US04831043

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