Potassium Carbonate → 4-(2-Piperidin-1-yl-ethoxy)-phenylamine

HRID 898524Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 898524
C(=O)([O-])[O-].[K+].[K+].[NH2:7][C:8]1[CH:13]=[CH:12][C:11]([OH:14])=[C:10](Cl)[CH:9]=1.Cl[CH2:17][CH2:18][N:19]1[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]1>C(#N)C>[N:19]1([CH2:18][CH2:17][O:14][C:11]2[CH:12]=[CH:13][C:8]([NH2:7])=[CH:9][CH:10]=2)[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 748271-(2-Chloroethyl)piperidineHCID 775784-Amino-2-chlorophenol

Produkt 1

HCID 30160254-(2-Piperidin-1-yl-ethoxy)-phenylamine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

15.4 g (111.00 mmol) of potassium carbonate was added to a solution of 4.0 g (27.86 mmol) of 4-amino-2-chlorophenol and 5.1 g (27.86 mmol) of 1-(2-chloro-ethyl)-piperidine in 50 mL acetonitrile and the mixture was stirred for 48 hours at RT. The solvent was evaporated off i. vac., the residue was combined with water and the aqueous phase was exhaustively extracted with EtOAc. The combined org. extracts were washed with water, dried over magnesium sulphate, evaporated down i. vac. and the residue was purified by column chromatography (silica gel, dichloromethane/MeOH/conc. aqueous ammonia 90:10:1).

Aufarbeitung

  1. customThe solvent was evaporated off i
  2. extractionthe aqueous phase was exhaustively extracted with EtOAc
  3. washextracts were washed with water
  4. dry with materialdried over magnesium sulphate
  5. customevaporated down i
  6. customand the residue was purified by column chromatography (silica gel, dichloromethane/MeOH/conc. aqueous ammonia 90:10:1)

Quellen und Nachweise

ORD-Eintrag
ord-9ff1f5c11f9f45ccbee9c2d8612370b8
Quelldatensatz
uspto-grants-2008_04
Patentnummer
US07351719B2

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