Fluorobenzene → HCID 19360812、化合物
反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl-].[Al+3].[Cl-].[Cl-].Cl[CH:13]([CH2:19]Cl)[CH2:14][Si:15]([Cl:18])([Cl:17])[Cl:16]>>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH:19]([C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=1[F:1])[CH2:13][CH2:14][Si:15]([Cl:18])([Cl:17])[Cl:16]参加物
4
実験手順
In the same apparatus and procedures as EXAMPLE 2 above, 18.8 ml (200 mmol) of fluorobenzene and 0.31 g (2.3 mmol) of aluminum chloride were alkylated with 5.61 g (22.8 mmol) of (2,3-dichloropropyl)trichlorosilane for 10 min at 70° C. The aluminum chloride catalyst was quenched with POCl3 and then stirred for another 1 hour 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 fluorobenzene were distilled, the reaction products were vacuum distilled to give 3.39 g of [3,3-bis(fluorophenyl)propyl]trichlorosilane (bp; 121-122° C./0.5 torr, yield; 41%) as a mixutre of isomers.
後処理
- customThe aluminum chloride catalyst was quenched with POCl3
- additionFreshly distilled hexane (50 ml) was added to the reaction mixture and insoluble solids in hexane
- filtrationwere filtered from the organic soultion
- distillationAfter hexane and fluorobenzene were distilled
- distillationdistilled
出典と根拠
- ORDレコード
- ord-1388c80601624ea082e75cff451879fa
- 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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