Dabco → HCID 21539297, Verbindung

HRID 1076227Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1076227
[CH2:1]1[C:6]2([C:15](=[S:16])[NH:14][C:8]3([CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]3)[NH:7]2)[CH2:5][CH2:4][CH2:3][CH2:2]1.[CH3:17][N:18]=[C:19]=[O:20].N12CCN(CC1)CC2>C1C=CC=CC=1>[CH3:17][NH:18][C:19]([N:14]1[C:15](=[S:16])[C:6]2([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5]2)[NH:7][C:8]21[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]2)=[O:20]

Komponenten

5

Edukt 3

HCID 9237DabcoHCID 12228Methyl Isocyanate2×HCID 853997NSC515893

Produkt 1

HCID 21539297HCID 21539297, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel

Versuchsvorschrift

4.8 Parts of 7,14-diazadispiro[5.1.5.2]pentadecane-15-thione, 2.28 parts of methyl isocyanate and a trace of 1,4-diazabicyclo[2.2.2]octane in 100 parts of dry benzene were heated at reflux for 4 days. A further 2.28 parts of methyl isocyanate were added and the solution again heated at reflux for 16 hours. The solvent was then evaporated in vacuo and the residue was crystallised twice from ethyl acetate to give 14-methylcarbamoyl-7,14-diazadispiro[5.1.5.2]pentadecane-15-thione as a colourless solid of melting point 127° to 129°C. This material gave the following elemental analysis by weight:

Aufarbeitung

  1. temperatureat reflux for 4 days
  2. temperaturethe solution again heated
  3. temperatureat reflux for 16 hours
  4. customThe solvent was then evaporated in vacuo
  5. customthe residue was crystallised twice from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-ad25879a620b44bdb3012342bd2e4636
Quelldatensatz
uspto-grants-1976_05
Patentnummer
US03956310

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