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Bromine → HCID 15580980, Verbindung

HRID 1759398
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1759398
O[CH:2]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[CH2:3][NH:4][C:5]([NH:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)=[S:6].BrBr>ClC(Cl)(Cl)Cl>[C:14]1([CH:2]2[N:7]3[C:5]([S:6][C:9]4[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=43)=[N:4][CH2:3]2)[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 24408BromineHCID 2873543HCID 2873543, Verbindung

Produkt 1

HCID 15580980HCID 15580980, VerbindungAusbeute 22 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 5943Carbon TetrachlorideLösungsmittel

Versuchsvorschrift

A mixture of 50 parts of N-(2-hydroxy-2-phenylethyl)-N'-phenylthiourea, 30 parts of bromine and 800 parts of tetrachloromethane is stirred and refluxed for 2 hours. The reaction mixture is evaporated. From the residue, the free base is liberated in the conventional manner with ammonium hydroxide and extracted with trichloromethane. The extract is dried, filtered and evaporated. The residue is suspended in boiling 4-methyl-2-pentanone. The product is filtered off and stirred in a diluted sodium hydroxide solution. The product is extracted with 4-methyl-2-pentanone. The extract is washed with water, dried, filtered and evaporated. The residue is crystallized from acetonitrile. The product is filtered off and dried, yielding 10 parts (22%) of 2,3-dihydro-3-phenylimidazo[2,1-b]benzothiazole; mp. 131.7° C.

Aufarbeitung

  1. temperaturerefluxed for 2 hours
  2. customThe reaction mixture is evaporated
  3. extractionextracted with trichloromethane
  4. customThe extract is dried
  5. filtrationfiltered
  6. customevaporated
  7. filtrationThe product is filtered off
  8. stirringstirred in a diluted sodium hydroxide solution
  9. extractionThe product is extracted with 4-methyl-2-pentanone
  10. washThe extract is washed with water
  11. customdried
  12. filtrationfiltered
  13. customevaporated
  14. customThe residue is crystallized from acetonitrile
  15. filtrationThe product is filtered off
  16. customdried

Quellen und Nachweise

ORD-Eintrag
ord-07648394f9e64f67b13fca2f9ae48bca
Quelldatensatz
uspto-grants-1982_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04340738

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