Acetic Acid → HCID 10398941, Verbindung

HRID 247646

Reaktionsgleichung

Reaktionsgleichung von HRID 247646
[CH2:1]([CH:3]1[CH2:8][CH2:7][CH2:6][CH2:5][C:4]1=O)[CH3:2].[CH3:10][C@@H:11]([NH2:18])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.C(O)(=O)C.O>C1(C)C=CC=CC=1>[CH3:10][C@H:11]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[N:18]=[C:4]1[CH2:5][CH2:6][CH2:7][CH2:8][CH:3]1[CH2:1][CH3:2]

Komponenten

6

Edukt 4

HCID 176Acetic AcidHCID 962WaterHCID 204742-EthylcyclohexanoneHCID 6431891-Phenethylamine, (+)-

Produkt 1

HCID 10398941HCID 10398941, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

A solution of 2-ethylcyclohexanone (6.92 mol, 873 g), (R)-α-methylbenzylamine (6.92 mol, 839 g), and 19.6 mL of acetic acid were refluxed for 12 hours under nitrogen in 2 L of toluene with azeotropic removal of water. The toluene was removed on a rotary evaporator and the product was divided into two portions. The unreacted 2-ethylcyclohexanone was distilled through a short path (bp 30° C., <10 mm), and the remainder of the product was then distilled through a 5" vacuum jacketed Vigreux column affording first a low melting solid (bp 80°-90° C. 23 mm), and then the product (bp 128°-133° C. 21.0 mm, 1.303 kg from both distillations combined, 5.68 mol, 82%).

Aufarbeitung

  1. customThe toluene was removed on a rotary evaporator
  2. distillationThe unreacted 2-ethylcyclohexanone was distilled through a short path (bp 30° C., <10 mm)
  3. distillationthe remainder of the product was then distilled through a 5" vacuum
  4. customaffording first a low melting solid (bp 80°-90° C. 23 mm)

Quellen und Nachweise

ORD-Eintrag
ord-35d3429614254b249873f0001b622e1f
Quelldatensatz
uspto-grants-1987_11
Patentnummer
US04709048

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