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(1,1'-Biphenyl)-4-carbonitrile → Hexachloroantimonate

HRID 2273503
ノート
印刷プレビュー

反応式

HRID 2273503 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([Br:11])[CH:10]=1)[C:5]([Cl:7])=[O:6].[C:12]1([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:17]=[CH:16][C:15]([C:18]#[N:19])=[CH:14][CH:13]=1.[Sb:26]([Cl:31])([Cl:30])([Cl:29])([Cl:28])[Cl:27]>C(Cl)(Cl)Cl>[C:12]1([C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)[CH:13]=[CH:14][C:15]([C:18]2[N:19]=[C:18]([C:15]3[CH:16]=[CH:17][C:12]([C:20]4[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=4)=[CH:13][CH:14]=3)[O+:6]=[C:5]([C:4]3[CH:3]=[C:2]([Br:1])[CH:10]=[C:9]([Br:11])[CH:8]=3)[N:19]=2)=[CH:16][CH:17]=1.[Cl:27][Sb-:26]([Cl:7])([Cl:31])([Cl:30])([Cl:29])[Cl:28]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 18021(1,1'-Biphenyl)-4-carbonitrileHCID 24294Antimony pentachlorideHCID 134505263,5-Dibromobenzoyl chloride

生成物 2

HCID 3695004HexachloroantimonateHCID 866699604,6-Bis(4-biphenylyl)-2-(3,5-dibromophenyl)-1,3,5-oxadiazin-1-ium

試薬・触媒・溶媒 1

HCID 6212
Chloroform
溶媒

反応条件

温度
0 °C

実験手順

2.98 g of 3,5-dibromobenzoyl chloride and 3.58 g of 4-biphenylcarbonitrile were dissolved in 40 mL of chloroform. The obtained solution was cooled to 0° C., and 2.99 g of antimony pentachloride was added dropwise to the cooled solution. The obtained mixed liquid was stirred at room temperature for 10 minutes, and then, heated under reflux for 14 hours. The obtained reaction mixture was cooled to room temperature, and then distilled under a reduced pressure to remove chloroform to give 4,6-bis(4-biphenylyl)-2-(3,5-dibromophenyl)-1,3,5-oxadiazin-1-ium=hexachloroantimonate as a red solid.

後処理

  1. additionThe obtained mixed liquid
  2. temperatureheated
  3. temperatureunder reflux for 14 hours
  4. customThe obtained reaction mixture
  5. temperaturewas cooled to room temperature
  6. distillationdistilled under a reduced pressure
  7. customto remove chloroform

出典と根拠

ORDレコード
ord-ba1c038a8b024af0ad4acf8aa9882bb3
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09120773B2

反応ノート

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