Triethylamine → HCID 21461086, Verbindung

HRID 1941444Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1941444
[C:1](Cl)(Cl)=[S:2].[CH2:5]([N:7]([CH2:14][CH2:15][CH2:16][NH2:17])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[CH3:6].C(N(CC)CC)C>C(Cl)Cl>[CH2:5]([N:7]([CH2:14][CH2:15][CH2:16][N:17]=[C:1]=[S:2])[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1)[CH3:6]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 10040ThiophosgeneHCID 3152197N-(3-Aminopropyl)-N-ethyl-N-phenylamine

Produkt 1

HCID 21461086HCID 21461086, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

A solution of thiophosgene (7.43 ml) in CH2Cl2 (300 ml) was added dropwise over 11/2 hours at 20° C. under a nitrogen atmosphere to a stirred solution of N-ethyl-N-(3-aminopropyl)aniline (17.8 g) and triethylamine (27.8 ml) in CH2Cl2 (500 ml). The mixture was stirred at 20° C. for a further 11/2 hours then heated under reflux for 11/2 hours. The mixture was allowed m cool washed with water, dried over MgSO4, filtered and solvent removed from the filtrate in vacuo. The product was purified by chromatography on silica gel eluting with CH2Cl2 to give N-ethyl-N-(3-isothiocyanatopropyl)aniline (72 g) as a red oil.

Aufarbeitung

  1. temperaturethen heated
  2. temperatureunder reflux for 11/2 hours
  3. temperaturecool
  4. washwashed with water
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. customsolvent removed from the filtrate in vacuo
  8. customThe product was purified by chromatography on silica gel eluting with CH2Cl2

Quellen und Nachweise

ORD-Eintrag
ord-f0a341d9b1c04104be7972bc29284dc9
Quelldatensatz
uspto-grants-1997_12
Patentnummer
US05703215

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