1,4-Dichlorobenzene → HCID 19360813、化合物

HRID 377050ノート

反応式

HRID 377050 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

HCID 19360813HCID 19360813、化合物収率 351.5%

試薬・触媒・溶媒 2

HCID 6451240Aluminum(III) Chloride触媒HCID 8058Hexane溶媒2 回

反応条件

温度
150 °C

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-6eeea1c50dd64498bdbc91225f48734c
出典データセット
uspto-grants-2000_02
特許番号
US06022987

反応ノート

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