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Potassium Phosphate, Tribasic → 6-Fluoro-4-nitrobiphenyl-3-carbonitrile

HRID 17531
ノート
印刷プレビュー

反応式

HRID 17531 の反応式
Br[C:2]1[C:3]([F:13])=[CH:4][C:5]([N+:10]([O-:12])=[O:11])=[C:6]([CH:9]=1)[C:7]#[N:8].[C:14]1(B(O)O)[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.P([O-])([O-])([O-])=O.[K+].[K+].[K+]>O1CCCC1.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>[F:13][C:3]1[C:2]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[CH:9][C:6]([C:7]#[N:8])=[C:5]([N+:10]([O-:12])=[O:11])[CH:4]=1
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 62657Potassium Phosphate, TribasicHCID 66827Phenylboronic AcidHCID 685846195-Bromo-4-fluoro-2-nitrobenzonitrile

生成物 1

HCID 685844646-Fluoro-4-nitrobiphenyl-3-carbonitrile

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒
HCID 8028
Tetrahydrofuran
溶媒

反応条件

温度
75 °C

実験手順

5-Bromo-4-fluoro-2-nitrobenzonitrile (I-240) (9.1 g, 37.14 mmol) was dissolved in tetrahydrofuran (270 ml), and at room temperature, phenylboronic acid (9.06 g, 74.28 mmol), tripotassium phosphate (15.77 g, 74.28 mmol) and tetrakis(triphenylphosphine)palladium (2.15 g, 1.86 mmol) were added. After stirred under nitrogen atmosphere at 75° C. for 48 hours, this was cooled to room temperature. The insoluble matter was separated by filtration, the filtrate was concentrated under reduced pressure. The residue was fractionated with chloroform and aqueous saturated ammonium chloride solution. The organic layer was washed with saturated brine, and dried over anhydrous sodium sulfate.

後処理

  1. temperaturethis was cooled to room temperature
  2. customThe insoluble matter was separated by filtration
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. washThe organic layer was washed with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate

出典と根拠

ORDレコード
ord-c16728b9ee0a48caa07a48e8b5a39f6b
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07737166B2

反応ノート

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