HCID 86697964, Verbindung → HCID 68360001, Verbindung

HRID 518796

Reaktionsgleichung

Reaktionsgleichung von HRID 518796
[I-].[CH3:2][N+:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:14]=[CH:13][C:12]([N+:15]([O-])=O)=[C:11]([O:18][CH:19]([CH3:21])[CH3:20])[CH:10]=2)=[CH:5][CH:4]=1.[H][H]>CO.O.[Pt]=O>[CH3:2][N:3]1[CH2:8][CH2:7][CH:6]([C:9]2[CH:14]=[CH:13][C:12]([NH2:15])=[C:11]([O:18][CH:19]([CH3:21])[CH3:20])[CH:10]=2)[CH2:5][CH2:4]1

Komponenten

5

Edukt 2

HCID 86697964HCID 86697964, VerbindungHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 68360001HCID 68360001, VerbindungAusbeute 96,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 86587499Platinum oxide monohydrateKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

A solution of 10 g of 1-methyl-4-[4-nitro-3-(propan-2-yloxy)phenyl]pyridinium iodide in 280 ml of methanol is hydrogenated in an autoclave on 2.9 g of platinum oxide hydrate, at a hydrogen pressure of 15 bar and at ambient temperature for 4 h. The catalyst is removed by filtration on Clarcel and the mixture is concentrated under vacuum. The residue is taken up in 200 ml of ethyl acetate and washed with 200 ml of 1M sodium hydroxide and then with a saturated sodium chloride solution. The organic phase is dried over magnesium sulfate and concentrated under vacuum, so as to obtain 6.0 g of 4-(1-methylpiperidin-4-yl)-2-(propan-2-yloxy)aniline.

Aufarbeitung

  1. customThe catalyst is removed by filtration on Clarcel
  2. concentrationthe mixture is concentrated under vacuum
  3. washwashed with 200 ml of 1M sodium hydroxide
  4. dry with materialThe organic phase is dried over magnesium sulfate
  5. concentrationconcentrated under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-946ca97885874ef1b5b284a4e52a64f0
Quelldatensatz
uspto-grants-2015_08
Patentnummer
US09115140B2

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