1,4-Dichlorobenzene → HCID 19360813, 화합물

HRID 377050노트

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HRID 377050 반응식
[Cl-:1].[Al+3].[Cl-:3].[Cl-].[Cl:5][C:6]1[CH:11]=[CH:10][C:9]([Cl:12])=[CH:8][CH:7]=1.Cl[CH:14]([Si:16]([CH3:19])([Cl:18])[Cl:17])Cl.O=P(Cl)(Cl)Cl>[Cl-].[Al+3].[Cl-].[Cl-].CCCCCC>[Cl:5][C:6]1[CH:11]=[CH:10][C:9]([Cl:12])=[CH:8][C:7]=1[CH:14]([Si:16]([CH3:19])([Cl:18])[Cl:17])[C:6]1[CH:11]=[C:10]([Cl:1])[CH:9]=[CH:8][C:7]=1[Cl:3]

참가 물질

7

반응물 4

HCID 46851,4-DichlorobenzeneHCID 24813Phosphorus oxychlorideHCID 73787Silane, dichloro(dichloromethyl)methyl-HCID 6451240Aluminum(III) Chloride

생성물 1

HCID 19360813HCID 19360813, 화합물수율 351.5%

시약·촉매·용매 2

HCID 6451240Aluminum(III) Chloride촉매HCID 8058Hexane용매2회

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온도
150 °C

실험 절차

To a 250 ml, three-necked, frame dried, round bottom flask equipped with a magnetic stirrer, a reflux condenser, and a dropping funnel, aluminum chloride 1.28 g (9.60 mmol) and 1,4-dichlorobenzene 62.89 g (428 mmol) were placed under dry nitrogen atmospheric pressure. After (dichloromethyl) methyldichlorosilane 14.12 g (72.31 mmol) was added to the solution, the reaction mixture was heated for 7 hours at 150° C. The aluminum chloride catalyst was quenched with POCl3 1.47 g (9.59 mmol) 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 at 0.2 torr to give 14.14 g of [bis(2,5-dichlorophenyl)methyl] methyldichlorosilane (bp; 154° C./0.2 torr, yield; 47%).

후처리

  1. customTo a 250 ml, three-necked, frame dried
  2. customround bottom flask equipped with a magnetic stirrer, a reflux condenser, and a dropping funnel
  3. filtrationwere filtered from the organic soultion
  4. distillationAfter hexane was distilled
  5. distillationdistilled at 0.2 torr

출처 및 근거

ORD 기록
ord-6eeea1c50dd64498bdbc91225f48734c
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06022987

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