Phosgene → HCID 178484191, Verbindung

HRID 67785

Reaktionsgleichung

Reaktionsgleichung von HRID 67785
C(Cl)([Cl:3])=O.O1CCCC1.[CH3:10][NH:11][C:12]([NH:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)=S>CN(C)C=O>[ClH:3].[CH3:10][NH:11][C:12]([Cl:3])=[N:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

Komponenten

5

Edukt 3

HCID 6371Phosgene2×HCID 8028TetrahydrofuranHCID 6982941-Methyl-3-phenylthiourea

Produkt 1

HCID 178484191HCID 178484191, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

After passing 6.3 g of phosgene into 40 ml of absolute tetrahydrofuran at room temperature, 8 g of 1-methyl-3-phenylthiourea are added, with stirring, the color of the suspension changing instantaneously to yellow. After adding 0.5 ml of dimethylformamide, the mixture is stirred for 20 hours at room temperature, nitrogen is then passed through the reaction mixture for about 30 minutes, in order to drive off the phosgene, and the crystals are filtered off and washed with tetrahydrofuran. Crystals with a melting point of 169° C. (with decomposition).

Aufarbeitung

  1. customat room temperature
  2. stirringthe mixture is stirred for 20 hours at room temperature
  3. filtrationthe crystals are filtered off
  4. washwashed with tetrahydrofuran

Quellen und Nachweise

ORD-Eintrag
ord-0f79ccd029194271bff947b0b7abc7ea
Quelldatensatz
uspto-grants-1982_08
Patentnummer
US04346088

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