Triethylamine → HCID 20403159, Verbindung

HRID 1758813Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1758813
[CH2:1]1[C:6]2([CH2:11][CH2:10][CH2:9][CH:8]=[CH:7]2)[CH2:5][CH2:4][CH2:3][NH:2]1.Br[CH2:13][CH2:14][OH:15].C(N(CC)CC)C>C1(C)C=CC=CC=1>[OH:15][CH2:14][CH2:13][CH:1]1[C:6]2([CH2:11][CH2:10][CH2:9][CH:8]=[CH:7]2)[CH2:5][CH2:4][CH2:3][NH:2]1

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 108982-BromoethanolHCID 20403147HCID 20403147, Verbindung

Produkt 1

HCID 20403159HCID 20403159, VerbindungAusbeute 72 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

A mixture of 2-azaspiro-[5.5]-undec-7-ene (30.2 g.; 0.20 mole), 2-bromoethanol (25 g.; 0.20 mole) and triethylamine (20.2 g.) in toluene (250 ml.) is heated under reflux for 5 hours. The solution is cooled, filtered to remove triethylamine hydrobromide and the filtrate concentrated under reduced pressure. The residual liquid was distilled under reduced pressure to afford 28 g. (72% yield) of 2-hydroxyethyl-2-azaspiro-[5.5]-undec-7-ene, b.p. 90°-91° C./0.45 mm.

Aufarbeitung

  1. temperatureis heated
  2. temperatureunder reflux for 5 hours
  3. temperatureThe solution is cooled
  4. filtrationfiltered
  5. customto remove triethylamine hydrobromide
  6. concentrationthe filtrate concentrated under reduced pressure
  7. distillationThe residual liquid was distilled under reduced pressure
  8. customto afford 28 g

Quellen und Nachweise

ORD-Eintrag
ord-6c6d029ad08e4cf49dd28c13c5d9522a
Quelldatensatz
uspto-grants-1983_02
Patentnummer
US04374991

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