Thiourea → HCID 22671284, Verbindung

HRID 1097359

Reaktionsgleichung

Reaktionsgleichung von HRID 1097359
[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[O:10][C:11]([F:14])([F:13])[F:12])[CH2:5]Br.NC(N)=[S:17]>C(O)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH2:5][SH:17])[CH:7]=[CH:8][C:9]=1[O:10][C:11]([F:14])([F:13])[F:12]

Komponenten

4

Versuchsvorschrift

To a solution of 3-chloro-4-(trifluoromethoxy)benzylbromide (5 g) in ethanol (100 ml) was added thiourea (5 g) and the mixture heated under reflux for 2 hours. The mixture was evaporated to dryness and the residue taken up into water (100 ml). To this solution was added sodium hydroxide pellets (3 g) and the mixture heated under reflux for 1 hour. The mixture was allowed to cool to room temperature and acidified with concentrated hydrochloric acid, the mixture was extracted with ether, dried and evaporated to give the subtitle compound as a colourless waxy solid (3.5 g).

Aufarbeitung

  1. temperaturethe mixture heated
  2. temperatureunder reflux for 2 hours
  3. customThe mixture was evaporated to dryness
  4. additionTo this solution was added sodium hydroxide pellets (3 g)
  5. temperaturethe mixture heated
  6. temperatureunder reflux for 1 hour
  7. extractionthe mixture was extracted with ether
  8. customdried
  9. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-bcf0365a16f44fd1ad39f5ee8d7eebb8
Quelldatensatz
uspto-grants-2012_03
Patentnummer
US08143261B2

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