1,3-Dichlorobenzene → HCID 12127967, Verbindung

HRID 377058

Reaktionsgleichung

Reaktionsgleichung von HRID 377058
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[CH:3]=1.[Cl-:9].[Al+3].[Cl-:11].[Cl-].Cl[CH:14]([Si:17]([Cl:20])([Cl:19])[Cl:18])[CH2:15]Cl>>[Cl:1][C:2]1[CH:3]=[C:4]([Cl:8])[CH:5]=[CH:6][C:7]=1[CH:15]([C:2]1[CH:7]=[CH:6][C:5]([Cl:9])=[CH:4][C:3]=1[Cl:11])[CH2:14][Si:17]([Cl:20])([Cl:19])[Cl:18]

Komponenten

4

Edukt 3

HCID 109431,3-DichlorobenzeneHCID 79093Silane, trichloro(1,2-dichloroethyl)-HCID 6451240Aluminum(III) Chloride

Produkt 1

HCID 12127967HCID 12127967, VerbindungAusbeute 187,2 %

Versuchsvorschrift

In the same apparatus and procedures as EXAMPLE 1 above, 49.1 ml (430 mmol) of 1,3-dichlorobenzene and 2.30 g (17.2 mmol) of aluminum chloride were alkylated with 19.40 g (83.5 mmol) of (1,2-dichloroethyl)trichlorosilane for 30 min at 120° C. The aluminum chloride catalyst was quenched with POCl3 and then stirred for another 1 hour to complete the deactivation. Freshly distilled hexane (100 ml) was added to the reaction mixture and insoluble solids in hexane were filtered from the organic soultion. After hexane was distilled, the reaction products were vacuum distilled to give 14.6 g of [2,2-bis(2,4-dichlorophenyl)ethyl]trichlorosilane (bp; 175-180° C./0.5 torr, yield; 39%).

Aufarbeitung

  1. customThe aluminum chloride catalyst was quenched with POCl3
  2. additionFreshly distilled hexane (100 ml) was added to the reaction mixture and insoluble solids in hexane
  3. filtrationwere filtered from the organic soultion
  4. distillationAfter hexane was distilled
  5. distillationdistilled

Quellen und Nachweise

ORD-Eintrag
ord-6deb113de3da4c4093a0c08eb6110b20
Quelldatensatz
uspto-grants-2000_02
Patentnummer
US06022987

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