1,2-Dichlorobenzene → HCID 19360819, 화합물

HRID 377062노트

반응식

HRID 377062 반응식
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]

참가 물질

4

반응물 3

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

생성물 1

HCID 19360819HCID 19360819, 화합물수율 114.2%

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-fe56d8eefea3416eaebcf01ed308094f
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06022987

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