1,2,3,4-Tetrachlorobenzene → [2,2-Bis(2,3,4,5-tetrachlorophenyl) ethyl]trichlorosilane

HRID 377059

반응식

HRID 377059 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[C:4]([Cl:9])[C:3]=1[Cl:10].[Cl-:11].[Al+3].[Cl-:13].[Cl-:14].Cl[CH:16]([Si:19]([Cl:22])([Cl:21])[Cl:20])[CH2:17]Cl>>[Cl:1][C:2]1[C:3]([Cl:10])=[C:4]([Cl:9])[C:5]([Cl:8])=[CH:6][C:7]=1[CH:17]([C:3]1[CH:4]=[C:5]([Cl:11])[C:6]([Cl:13])=[C:7]([Cl:14])[C:2]=1[Cl:1])[CH2:16][Si:19]([Cl:22])([Cl:21])[Cl:20]

참가 물질

4

반응물 3

HCID 124631,2,3,4-TetrachlorobenzeneHCID 79093Silane, trichloro(1,2-dichloroethyl)-HCID 6451240Aluminum(III) Chloride

생성물 1

HCID 53867974[2,2-Bis(2,3,4,5-tetrachlorophenyl) ethyl]trichlorosilane수율 220.1%

실험 절차

In the same apparatus and procedures as EXAMPLE 1 above, 43.18 g (200 mmol) of 1,2,3,4-tetrachlorobenzene and 1.07 g (8.0 mmol) of aluminum chloride were alkylated with 9.30 g (40.0 mmol) of (1,2-dichloroethyl)trichlorosilane for 10 min at 130° C. The aluminum chloride catalyst was quenched with POCl3 and then stirred for another 30 min 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 10.41 g of [2,2-bis(2,3,4,5-tetrachlorophenyl) ethyl]trichlorosilane (bp; 218-222° C./0.5 torr, yield; 44%).

후처리

  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

출처 및 근거

ORD 기록
ord-005acce036c24ac3af248b0103f6e476
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06022987

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