Tert-Butylamine → 2-(4-Amino-3-chloro-5-trifluoromethylphenyl)-2-tert-butylaminoethanol

HRID 11899

Reaktionsgleichung

Reaktionsgleichung von HRID 11899
[NH2:1][C:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][C:5]([CH:12]2[O:14][CH2:13]2)=[CH:4][C:3]=1[Cl:15].[C:16]([NH2:20])([CH3:19])([CH3:18])[CH3:17]>C(O)C>[NH2:1][C:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][C:5]([CH:12]([NH:20][C:16]([CH3:19])([CH3:18])[CH3:17])[CH2:13][OH:14])=[CH:4][C:3]=1[Cl:15]

Komponenten

4

Edukt 2

HCID 6385Tert-ButylamineHCID 15067147(4-Amino-3-chloro-5-trifluoromethyl-phenyl)-ethylene oxide

Produkt 1

HCID 99977892-(4-Amino-3-chloro-5-trifluoromethylphenyl)-2-tert-butylaminoethanolAusbeute 20 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

5.2 g (0.022 mol) of (4-amino-3-chloro-5-trifluoromethyl-phenyl)-ethylene oxide was dissolved in 26 ml of anhydrous ethanol and treated with 5.1 ml (0.049 mol) of tert-butylamine. The mixture was refluxed for 13 h, and then evaporated. The residue was extracted with 2N hydrochloric acid for several times. Aqueous layers were combined and extracted with toluene and treated with activated carbon. The pH was adjusted to 10 with 20% sodium hydroxide solution. The precipitate was collected by filtration, 2-(4-amino-3-chloro-5-trifluoromethylphenyl)-2-tert-butylaminoethanol was obtained. Yield 20–30%; melting point 85–90° C.

Aufarbeitung

  1. temperatureThe mixture was refluxed for 13 h
  2. customevaporated
  3. extractionThe residue was extracted with 2N hydrochloric acid for several times
  4. extractionextracted with toluene
  5. additiontreated with activated carbon
  6. filtrationThe precipitate was collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-5946892308ac4131bb6fd116f5fb02cd
Quelldatensatz
uspto-grants-2006_08
Patentnummer
US07098364B2

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