Triethylamine → HCID 21545008, Verbindung

HRID 1605804Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1605804
[CH3:1][S:2]([C:5]1[S:6][C:7]([N:10]([CH3:14])[C:11](Cl)=[O:12])=[N:8][N:9]=1)(=[O:4])=[O:3].[O:15]1[CH2:20][CH2:19][CH2:18][O:17][CH:16]1[CH2:21][NH2:22].C(N(CC)CC)C>C1C=CC=CC=1>[CH3:1][S:2]([C:5]1[S:6][C:7]([N:10]([CH3:14])[C:11]([NH:22][CH2:21][CH:16]2[O:17][CH2:18][CH2:19][CH2:20][O:15]2)=[O:12])=[N:8][N:9]=1)(=[O:4])=[O:3]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 212488031-(1,3-Dioxan-2-yl)methanamineHCID 21544998HCID 21544998, Verbindung

Produkt 1

HCID 21545008HCID 21545008, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel

Versuchsvorschrift

N-(2-Methylsulfonyl-1,3,4-thiadiazol-5-yl)-N-methylcarbamoyl chloride (0.05 mole), N-(1,3-dioxan-2-ylmethyl)amine (0.05 mole), triethylamine (0.07 mole) and benzene (200 ml) are charged into a glass reaction vessel equipped with a mechanical stirrer, thermometer and reflux condenser. The reaction mixture is then heated at reflux for a period of about 4 hours. After this time the mixture is cooled to room temperature and is filtered. The filtrate is washed with water and is dried over anhydrous magnesium sulfate. The dried solution is then stripped of solvent under reduced pressure to yield the desired product N-(2-methylsulfonyl-1,3,4-thiadiazol-5-yl)-N-methyl-N'-(1,3-dioxan-2-ylmethyl)urea.

Aufarbeitung

  1. customequipped with a mechanical stirrer
  2. temperaturethermometer and reflux condenser
  3. temperatureThe reaction mixture is then heated
  4. temperatureat reflux for a period of about 4 hours
  5. filtrationis filtered
  6. washThe filtrate is washed with water
  7. dry with materialis dried over anhydrous magnesium sulfate

Quellen und Nachweise

ORD-Eintrag
ord-5f72656f54184a46a7fe6c815f28720d
Quelldatensatz
uspto-grants-1976_04
Patentnummer
US03951640

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