1,4-Dichlorobenzene → [2,2-Bis(2,5-dichlorophenyl)ethyl]trichlorosilane

HRID 377057

反応式

HRID 377057 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][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:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[CH:15]([C:2]1[CH:7]=[C:6]([Cl:9])[CH:5]=[CH:4][C:3]=1[Cl:11])[CH2:14][Si:17]([Cl:20])([Cl:19])[Cl:18]

参加物

4

反応物 3

HCID 46851,4-DichlorobenzeneHCID 79093Silane, trichloro(1,2-dichloroethyl)-HCID 6451240Aluminum(III) Chloride

生成物 1

HCID 12127968[2,2-Bis(2,5-dichlorophenyl)ethyl]trichlorosilane収率 287.3%

実験手順

In the same apparatus and procedures as EXAMPLE 2 above, 17.35 g (118 mmol) of 1,4-dichlorobenzene and 0.47 g (3.5 mmol) of aluminum chloride were alkylated with 5.45 g (23.5 mmol) of (1,2-dichloroethyl)trichlorosilane for 20 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 (50 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 4.56 g of [2,2-bis(2,5-dichlorophenyl)ethyl]trichlorosilane (bp; 161-163° C./0.5 torr, yield; 43%).

後処理

  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 was distilled
  5. distillationdistilled

出典と根拠

ORDレコード
ord-2cb30ef98a9441a097f67064c95734ae
出典データセット
uspto-grants-2000_02
特許番号
US06022987

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