ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Sodium Carbonate → 1,1':4',1''-Terphenyl, 4-iodo-

HRID 1828405
ノート
印刷プレビュー

反応式

HRID 1828405 の反応式
I[C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][C:11]([I:14])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.[C:15]1(OB(O)O)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.C(=O)([O-])[O-].[Na+].[Na+]>C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C1(C)C=CC=CC=1>[I:14][C:11]1[CH:12]=[CH:13][C:8]([C:5]2[CH:6]=[CH:7][C:2]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)=[CH:3][CH:4]=2)=[CH:9][CH:10]=1
参加物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 10340Sodium CarbonateHCID 763484,4'-Diiodo-1,1'-biphenylHCID 78412Phenyl dihydrogen orthoborate

生成物 1

HCID 111110491,1':4',1''-Terphenyl, 4-iodo-収率 35%

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒
HCID 1140
Toluene
溶媒

実験手順

The compound was prepared under Suzuki reaction conditions. 4,4′-diiodo-biphenyl (1.0 g, 2.46 mmol), phenyl boric acid (0.24 g, 1.970 mmol), tetrakis(triphenylphosphine)palladium (0.085 g, 0.074 mmol), 2M-sodium carbonate (12.3 ml) and toluene (76 ml) were simultaneously mixed, freezed under liquid nitrogen, evacuated by a vacuum pump and then warmed to room temperature to be melted. This procedure was repeated twice, followed by injection of nitrogen. The mixed solution was refluxed for 2 days and cooled to room temperature. Thereafter, a small amount of distilled water was added, and the organic layer was filtered three times with dichloromethane, dried with sodium sulfate. Then, the dichloromethane was concentrated under reduced pressure. Purification by silica gel chromatography using 1% dichloromethane in hexane gave 4″-iodo-[1,1′;4′,1″]terphenyl (Yield: 0.245 g, 35%). The structure of the product was identified through the NMR spectrum and mass spectrum. FIG. 6 shows the mass spectrum of 4″-iodo-[1,1′;4′,1″]terphenyl.

後処理

  1. customThe compound was prepared under Suzuki reaction conditions
  2. customevacuated by a vacuum pump
  3. temperatureThe mixed solution was refluxed for 2 days
  4. temperaturecooled to room temperature
  5. additionThereafter, a small amount of distilled water was added
  6. filtrationthe organic layer was filtered three times with dichloromethane
  7. dry with materialdried with sodium sulfate
  8. concentrationThen, the dichloromethane was concentrated under reduced pressure
  9. customPurification by silica gel chromatography

出典と根拠

ORDレコード
ord-3722f70ca65948e3a50a4c1cb04e2068
出典データセット
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07057074B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート