Carbon Dioxide → N-(2,6-Diethyl-phenyl)-N'-tert.-butyl-thiourea

HRID 1701561Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1701561
[CH2:1]([C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([CH2:9][CH3:10])[C:4]=1[N:11]=[C:12]=[S:13])[CH3:2].C([C:16]1C=CC=[C:19](CC)[C:17]=1[NH2:18])C.[C:25](=O)([O-])[O-].[Ca+2].C(Cl)(Cl)=S.C(=O)=O>C(Cl)Cl.O>[CH2:1]([C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([CH2:9][CH3:10])[C:4]=1[NH:11][C:12]([NH:18][C:17]([CH3:19])([CH3:25])[CH3:16])=[S:13])[CH3:2]

Komponenten

8

Edukt 5

HCID 280Carbon DioxideHCID 10040ThiophosgeneHCID 10112Calcium CarbonateHCID 113692,6-DiethylanilineHCID 1411932,6-Diethylphenyl isothiocyanate

Produkt 1

HCID 20346927N-(2,6-Diethyl-phenyl)-N'-tert.-butyl-thiourea

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

2,6-Diethyl-phenyl isothiocyanate can be prepared as follows: 100 g of 2,6-diethylaniline in 200 ml of methylene chloride are added dropwise at 0°-5°, whilst stirring, to a mixture of 500 ml of methylene chloride, 300 ml of water, 120 g of calcium carbonate and 92 g of thiophosgene. The mixture is then heated to the reflux temperature until the evolution of CO2 has ended. The cooled batch is filtered and the methylene chloride layer is separated off, dried with calcium chloride and fractionated.

Aufarbeitung

  1. filtrationThe cooled batch is filtered
  2. customthe methylene chloride layer is separated off
  3. dry with materialdried with calcium chloride

Quellen und Nachweise

ORD-Eintrag
ord-f9f97215daf94e67ae5df4197d44dfa3
Quelldatensatz
uspto-grants-1980_03
Patentnummer
US04194008

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