Triethylamine → HCID 54342534, Verbindung

HRID 1076189Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1076189
[NH:1]=[C:2]1[N:6]=[C:5]([N:7]([CH3:9])[CH3:8])[S:4][S:3]1.[C:10]([N:14]=[C:15]=[O:16])([CH3:13])([CH3:12])[CH3:11].C(N(CC)CC)C>O1CCCC1>[C:10]([NH:14][C:15]([N:1]=[C:2]1[N:6]=[C:5]([N:7]([CH3:9])[CH3:8])[S:4][S:3]1)=[O:16])([CH3:13])([CH3:12])[CH3:11]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 62412tert-Butyl isocyanateHCID 215392483-imino-5-dimethylamino-3H-1,2,4-dithiazole

Produkt 1

HCID 54342534HCID 54342534, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A suspension of 4.75 parts of the hydrobromide salt of 3-imino-5-dimethylamino-3H-1,2,4-dithiazole, two parts of t-butyl isocyanate, two parts of triethylamine, and 50 parts of tetrahydrofuran was stirred and refluxed for two days. The reaction mixture was cooled and the insoluble triethylammonium bromide was removed by filtration and discarded. The filtrate was then evaporated under reduced pressure leaving a white solid, which was recrystallized from isopropanol to afford 3.4 parts of 1-t-butyl-3-(5-dimethylamino-3H-1,2,4-dithiazol-3-ylidene)urea, m.p. 174°-177°C. dec.

Aufarbeitung

  1. temperaturerefluxed for two days
  2. temperatureThe reaction mixture was cooled
  3. customthe insoluble triethylammonium bromide was removed by filtration
  4. customThe filtrate was then evaporated under reduced pressure
  5. customleaving a white solid, which
  6. customwas recrystallized from isopropanol

Quellen und Nachweise

ORD-Eintrag
ord-28ba2993189e456fb673467b2f17fa9c
Quelldatensatz
uspto-grants-1976_05
Patentnummer
US03956303

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