Biphenyl → HCID 11129642, 화합물

HRID 1457370노트

반응식

HRID 1457370 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[C:5]1([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.Cl[CH:18]([Si:20]([CH3:23])([Cl:22])[Cl:21])Cl.O=P(Cl)(Cl)Cl>[Cl-].[Al+3].[Cl-].[Cl-].CCCCCC>[CH3:18][Si:20]([Cl:22])([Cl:21])[CH:23]1[C:16]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[C:5]2[C:10]1=[CH:9][CH:8]=[CH:7][CH:6]=2

참가 물질

7

반응물 4

HCID 7095BiphenylHCID 24813Phosphorus oxychlorideHCID 73787Silane, dichloro(dichloromethyl)methyl-HCID 6451240Aluminum(III) Chloride

생성물 1

HCID 11129642HCID 11129642, 화합물수율 59%

시약·촉매·용매 2

HCID 6451240Aluminum(III) Chloride촉매HCID 8058Hexane용매2회

실험 절차

To a 100 ml, three-necked, frame dried, round bottom flask equipped with a magnetic stirrer, a reflux condenser, and a dropping funnel, aluminum chloride 1.43 g (10.7 mmol) and biphenyl 16.5 g (107 mmol) were placed under dry nitrogen atmospheric pressure. After (dichloromethyl)methyldichlorosilane 7.50 ml (53.5 mmol) was added to the solution, the reaction mixture was heated for 2.5 hrs. at 120° C. The aluminum chloride catalyst was quenched with POCl3 1.04 ml (11.2 mmol) and then stirred for another 1 hr. 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 solution. After hexane was distilled, the reaction products were vacuum distilled at 0.2 torr to give 8.79 g of 9-(methyldichlorosilyl)fluorene (bp; 115°-120° C./0.2 torr, yield; 59%).

후처리

  1. customTo a 100 ml, three-necked, frame dried
  2. customround bottom flask equipped with a magnetic stirrer, a reflux condenser, and a dropping funnel
  3. temperaturethe reaction mixture was heated for 2.5 hrs
  4. customat 120° C
  5. filtrationwere filtered from the organic solution
  6. distillationAfter hexane was distilled
  7. distillationdistilled at 0.2 torr

출처 및 근거

ORD 기록
ord-8048e98e56424bcf9cef3f14c1838a1b
출처 데이터셋
uspto-grants-1998_12
특허 번호
US05847182

반응 노트

불러오는 중…