4,4'-Dichlorobenzhydrol → 4,4'-Dichlorobenzhydryl chloride

HRID 231212

Reaktionsgleichung

Reaktionsgleichung von HRID 231212
S(Cl)([Cl:3])=O.[Cl:5][C:6]1[CH:20]=[CH:19][C:9]([CH:10](O)[C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][CH:12]=2)=[CH:8][CH:7]=1>>[Cl:5][C:6]1[CH:20]=[CH:19][C:9]([CH:10]([Cl:3])[C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][CH:12]=2)=[CH:8][CH:7]=1

Komponenten

3

Versuchsvorschrift

Forty-two milliliters of thionyl chloride were gradually added to 75 g of 4,4'-dichlorobenzhydrol. When the addition was complete, the reaction was heated on a steam bath for 2 hours. The excess thionyl chloride was removed in vacuo. One hundred milliliters of carbon tetrachloride were added, and the solvent was again evaporated. The carbon tetrachloride treatment was repeated and upon evaporation the resulting oil was crystallized from petroleum ether to provide 65.3 g of the desired sub-titled intermediate, m.p. 63° C.

Aufarbeitung

  1. additionWhen the addition
  2. temperaturethe reaction was heated on a steam bath for 2 hours
  3. customThe excess thionyl chloride was removed in vacuo
  4. additionOne hundred milliliters of carbon tetrachloride were added
  5. customthe solvent was again evaporated
  6. customThe carbon tetrachloride treatment was repeated and upon evaporation the resulting oil
  7. customwas crystallized from petroleum ether

Quellen und Nachweise

ORD-Eintrag
ord-816a8a416f95473299bb77d8e4cf6ead
Quelldatensatz
uspto-grants-1989_07
Patentnummer
US04845227

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