1,2-Dichlorobenzene → HCID 19360819, Verbindung

HRID 377062Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 377062
Cl[C:2]1[C:7]([Cl:8])=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl-:9].[Al+3].[Cl-:11].[Cl-:12].Cl[CH:14]([CH:20](Cl)[CH3:21])[CH2:15][Si:16]([Cl:19])([Cl:18])[Cl:17]>>[Cl:9][C:2]1[CH:7]=[C:6]([Cl:11])[CH:5]=[CH:4][C:3]=1[C:20]([C:2]1[CH:3]=[CH:4][C:5]([Cl:12])=[CH:6][C:7]=1[Cl:8])([CH3:21])[CH2:14][CH2:15][Si:16]([Cl:19])([Cl:18])[Cl:17]

Komponenten

4

Edukt 3

HCID 72391,2-DichlorobenzeneHCID 6451240Aluminum(III) ChlorideHCID 19360811Trichloro(2,3-dichlorobutyl)silane

Produkt 1

HCID 19360819HCID 19360819, VerbindungAusbeute 114,2 %

Versuchsvorschrift

In the same apparatus and procedures as EXAMPLE 2 above, 26.3 ml (230 mmol) of 2,3-dichlorobenzene and 1.23 g (9.2 mmol) of aluminum chloride were alkylated with 11.91 g (45.7 mmol) of (2,3-dichlorobutyl)trichlorosilane for 20 min at 90° C. The aluminum chloride catalyst was quenched with POCl3 and then stirred for another 30 min to complete the deactivation. Freshly distilled hexane (50 ml) was added to the reaction mixture and insoluble solids in hexane were filtered from the organic soultion. After hexane and benzene were distilled, the reaction products were vacuum distilled to give 5.06 g of [3,3-bis(2,4-dichlorophenyl)butyl]trichlorosilane (bp; 186-190° C./0.5 torr, yield; 23%).

Aufarbeitung

  1. customThe aluminum chloride catalyst was quenched with POCl3
  2. additionFreshly distilled hexane (50 ml) was added to the reaction mixture and insoluble solids in hexane
  3. filtrationwere filtered from the organic soultion
  4. distillationAfter hexane and benzene were distilled
  5. distillationdistilled

Quellen und Nachweise

ORD-Eintrag
ord-fe56d8eefea3416eaebcf01ed308094f
Quelldatensatz
uspto-grants-2000_02
Patentnummer
US06022987

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