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4,4'-Dichlorodiphenylmethane → 1,1'-(4-Chlorobutane-1,1-diyl)bis(4-chlorobenzene)

HRID 1700940
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1700940
[CH:1]1[C:6]([CH2:7][C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=2)=[CH:5][CH:4]=[C:3]([Cl:15])[CH:2]=1.C([Li])CCC.[Cl:21][CH2:22][CH2:23][CH2:24]I>O1CCCC1>[Cl:21][CH2:22][CH2:23][CH2:24][CH:7]([C:8]1[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=1)[C:6]1[CH:1]=[CH:2][C:3]([Cl:15])=[CH:4][CH:5]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 75764,4'-DichlorodiphenylmethaneHCID 813631-Chloro-3-iodopropaneHCID 178418339Butyllithium

Produkt 1

HCID 183190411,1'-(4-Chlorobutane-1,1-diyl)bis(4-chlorobenzene)Ausbeute 44 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

A solution of 4,4′-dichlorodiphenylmethane (4.37 g, 18.4 mmol) (Blackwell, J. et all, J. Chem. Soc., 1961, 1405) in dry tetrahydrofuran (50 ml) was treated at 0° C. with butyllithium (12.1 ml of 1.6 M, 19.36 mmol) added dropwise over 15 min. After 15 min, the red solution was then added dropwise to a cold (−78° C.) solution of 1-chloro-3-iodopropane (15.0 g, 73.4 mmol) in dry tetrahydrofuran (120 ml). After 20 min at −78° C., the reaction mixture was quenched by the addition of saturated ammonium chloride (100 ml) and diluted with toluene. The organic phase was washed with brine and dried. The oil obtained after evaporation of the solvent was purified on silica gel (elution hexane-toluene 85:15) and distilled under vacuum to give 2.54 g (44%) of the title material as a clear oil: bp 110-130° C./1.5 torr (air bath temperature).

Aufarbeitung

  1. additionadded dropwise over 15 min
  2. waitAfter 20 min at −78° C.
  3. customthe reaction mixture was quenched by the addition of saturated ammonium chloride (100 ml)
  4. additiondiluted with toluene
  5. washThe organic phase was washed with brine
  6. customdried
  7. customThe oil obtained
  8. customafter evaporation of the solvent
  9. customwas purified on silica gel (elution hexane-toluene 85:15)
  10. distillationdistilled under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-4906f058dea0494c8e6b83d9991829bf
Quelldatensatz
uspto-grants-2002_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06350892B1

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