Methanol → HCID 19832480, Verbindung

HRID 2051584

Reaktionsgleichung

Reaktionsgleichung von HRID 2051584
[C:1]1([NH:7][C:8]2[CH:13]=[CH:12][C:11]([NH:14][CH:15]([CH3:20])[CH2:16][CH:17]([CH3:19])[CH3:18])=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.N1CCCC1.[C:26]([O-])([O-])=[O:27].[K+].[K+].[C:32](Cl)(Cl)=[S:33].CO>C(Cl)(Cl)Cl>[CH3:26][O:27][C:32](=[S:33])[N:14]([C:11]1[CH:12]=[CH:13][C:8]([NH:7][C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[CH:9][CH:10]=1)[CH:15]([CH3:20])[CH2:16][CH:17]([CH3:19])[CH3:18]

Komponenten

7

Edukt 5

HCID 887MethanolHCID 10040ThiophosgeneHCID 11430Potassium CarbonateHCID 131011,4-Benzenediamine, N-(1,3-dimethylbutyl)-N'-phenyl-HCID 31268Pyrrolidine

Produkt 1

HCID 19832480HCID 19832480, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel2×

Versuchsvorschrift

N-phenyl-N'-(1,3-dimethylbutyl)-p-phenylenediamine (26.8g, 0.10 mol) in 100 mL chloroform and 30g (0.22 mol) of K2CO3 as a saturated aqueous solution are placed in a 250 mL, 3-neck round bottom flask. Thiophosgene (11.5g: 0.10 mol) in 20 mL chloroform is added at such a rate sufficient to reach and maintain reflux conditions. Stirring is continued until the mixture returns to room temperature. Methanol (6.4g, 0.2 mol) is then added and the mixture refluxed for 4 hours. The organic layer is separated, dried with MgSO4 and the solvent removed on a rotary evaporator to give the desired product.

Aufarbeitung

  1. temperaturemaintain
  2. temperaturereflux conditions
  3. customreturns to room temperature
  4. temperaturethe mixture refluxed for 4 hours
  5. customThe organic layer is separated
  6. dry with materialdried with MgSO4
  7. customthe solvent removed on a rotary evaporator

Quellen und Nachweise

ORD-Eintrag
ord-0d6a7e843f8543d29cec7e28e8e1f0d9
Quelldatensatz
uspto-grants-1991_05
Patentnummer
US05019611

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