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1-Bromopropane → HCID 178460859, Verbindung

HRID 260724
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 260724
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][NH:9][C:10]([NH2:12])=[S:11].[CH2:13](Br)[CH2:14][CH3:15]>C(#N)C>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][NH:9][C:10](=[NH:12])[S:11][CH2:13][CH2:14][CH3:15]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 78401-BromopropaneHCID 22400378HCID 22400378, Verbindung

Produkt 1

HCID 178460859HCID 178460859, VerbindungAusbeute 78 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

A mixture of 1-(2-chlorophenyl)methyl thiourea (3 g, 14.9 mmol) and propylbromide (13.5 g, 110 mmol) in acetonitrile (20 mL) was refluxed for 5 hours. The solvent was evaporated, the residue was dissolved in 200 mL of 50% water/ether and acidified with 48% hydrobromic acid solution. The two phases were separated, the aqueous layer was washed with ether and then the aqueous layer was basified with 10% sodium carbonate solution. The liberated product was extracted with diethyl ether, washed with water and brine, dried and concentrated to give 1-(2-chlorophenyl)methyl-2-propyl-2-thiopseudourea (2.82 g, 78%); mp 112°-114° C.

Aufarbeitung

  1. temperaturewas refluxed for 5 hours
  2. customThe solvent was evaporated
  3. dissolutionthe residue was dissolved in 200 mL of 50% water/ether
  4. customThe two phases were separated
  5. washthe aqueous layer was washed with ether
  6. extractionThe liberated product was extracted with diethyl ether
  7. washwashed with water and brine
  8. customdried
  9. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-629220f6940f4c29a1fb10c7dd7dc1b0
Quelldatensatz
uspto-grants-1996_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05530017

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