Thionyl Chloride → HCID 13105626, Verbindung

HRID 354947

Reaktionsgleichung

Reaktionsgleichung von HRID 354947
[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][C:5]([NH:9][CH2:10][CH2:11][CH2:12]O)=[C:4]([N+:14]([O-:16])=[O:15])[CH:3]=1.S(Cl)([Cl:19])=O>ClC(Cl)Cl>[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][C:5]([NH:9][CH2:10][CH2:11][CH2:12][Cl:19])=[C:4]([N+:14]([O-:16])=[O:15])[CH:3]=1

Komponenten

4

Edukt 2

HCID 24386Thionyl ChlorideHCID 1129553-((4,5-Dichloro-2-nitrophenyl)amino)-1-propanol

Produkt 1

HCID 13105626HCID 13105626, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

To a stirred mixture of 10 parts of 3-[(4,5-dichloro-2-nitrophenyl)amino]-1-propanol and 75 parts of trichloromethane are added dropwise 11.2 parts of sulfinyl chloride. Upon completion, stirring is continued for 4 hours at reflux temperature. The reaction mixture is evaporated and the residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (98:2) as eluent. The pure fractions are collected and the eluent is evaporated. The residue is crystallized from 2,2'-oxybispropane. The product is filtered off and dried, yielding 4,5-dichloro-N-(3-chloropropyl)-2-nitrobenzenamine; mp. 78° C.

Aufarbeitung

  1. temperatureat reflux temperature
  2. customThe reaction mixture is evaporated
  3. customthe residue is purified by column-chromatography over silica gel using
  4. additiona mixture of trichloromethane and methanol (98:2) as eluent
  5. customThe pure fractions are collected
  6. customthe eluent is evaporated
  7. customThe residue is crystallized from 2,2'-oxybispropane
  8. filtrationThe product is filtered off
  9. customdried

Quellen und Nachweise

ORD-Eintrag
ord-21b05452eba24d8784dfac9975561586
Quelldatensatz
uspto-grants-1983_03
Patentnummer
US04377578

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