Potassium Carbonate → 2-[(p-phenoxy)phenoxy]ethylthiocarbamic acid S-ethyl ester

HRID 2058269Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2058269
[O:1]([C:8]1[CH:17]=[CH:16][C:11]([O:12][CH2:13][CH2:14][NH2:15])=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:18]([S:20][C:21](Cl)=[O:22])[CH3:19].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH2:18]([S:20][C:21](=[O:22])[NH:15][CH2:14][CH2:13][O:12][C:11]1[CH:16]=[CH:17][C:8]([O:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)=[CH:9][CH:10]=1)[CH3:19]

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 18056Ethyl chlorothioformateHCID 110316512-(4-Phenoxyphenoxy)ethanamine

Produkt 1

HCID 127696972-[(p-phenoxy)phenoxy]ethylthiocarbamic acid S-ethyl esterAusbeute 53 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

4 g of 2-[(p-phenoxy)phenoxy]ethylamine and 11.2 g of chlorothioformic acid S-ethyl ester are dissolved in 150 ml of acetone. 14.5 g of potassium carbonate are added to the solution. This mixture is heated under reflux for 6 hours and then filtered. The residue is washed with acetone and the filtrate is evaporated in vacuo. The crystalline residue is suspended in cyclohexane and filtered to yield 2.5 g (53%) of 2-[(p-phenoxy)phenoxy]ethylthiocarbamic acid S-ethyl ester, m.p.--56°-58° C.

Aufarbeitung

  1. temperatureThis mixture is heated
  2. temperatureunder reflux for 6 hours
  3. filtrationfiltered
  4. washThe residue is washed with acetone
  5. customthe filtrate is evaporated in vacuo
  6. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-c5fee56d1f014410a0af56bca5b63bfd
Quelldatensatz
uspto-grants-1980_07
Patentnummer
US04215139

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