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Tris(1,1-dimethylethyl)phosphine → 4,2'-Difluoro-5'-nitrobiphenyl-2-carbonitrile

HRID 1167120
ノート
印刷プレビュー

反応式

HRID 1167120 の反応式
Br[C:2]1[CH:9]=[CH:8][C:7]([F:10])=[CH:6][C:3]=1[C:4]#[N:5].[F:11][C:12]1[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[CH:14][C:13]=1B1OC(C)(C)C(C)(C)O1.[F-].[K+].C(P(C(C)(C)C)C(C)(C)C)(C)(C)C>O1CCCC1.O.O1CCOCC1.[OH-].[Na+].C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[F:10][C:7]1[CH:6]=[C:3]([C:4]#[N:5])[C:2]([C:13]2[CH:14]=[C:15]([N+:18]([O-:20])=[O:19])[CH:16]=[CH:17][C:12]=2[F:11])=[CH:9][CH:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 4

HCID 83681Tris(1,1-dimethylethyl)phosphineHCID 936542-Bromo-5-fluorobenzonitrileHCID 522689Potassium FluorideHCID 38332972-Fluoro-5-nitrophenylboronic acid, pinacol ester

生成物 1

HCID 112424114,2'-Difluoro-5'-nitrobiphenyl-2-carbonitrile収率 108%

試薬・触媒・溶媒 5

HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 962Water溶媒
HCID 8028Tetrahydrofuran溶媒
HCID 14798Sodium Hydroxide溶媒
HCID 312751,4-Dioxane溶媒

実験手順

A mixture of 2-bromo-5-fluorobenzonitrile (20 g, 100 mmol), 2-(2-fluoro-5-nitrophenyl)-4,4,5,5-tetramethyl-[1,3,2]dioxaborolane (from Example B) (34.7 g, 130 mmol) and potassium fluoride (19.2 g, 330 mmol) in tetrahydrofuran (350 ml) and water (20 ml) was degassed with nitrogen for 30 min then treated with tris(dibenzylideneacetone)dipalladium(0) (1.83 g, 2 mmol) followed by tri-tert-butylphosphine (4 ml of a 0.2 M solution in 1,4-dioxane, 0.8 mmol). This mixture was stirred at ambient temperature for 30 min before heating at 50° C. for 18 h. The resulting dark suspension was cooled to ambient temperature, diluted with 0.5 M sodium hydroxide (2.5 l) and stirred at ambient temperature for 4 h. The solid was collected by filtration, washed with water and dried under suction to afford 4,2′-difluoro-5′-nitrobiphenyl-2-carbonitrile as a black solid (28.1 g, >100%) contaminated with dibenzylideneacetone: 1H NMR (360 MHz, CDCl3) δ 7.38-7.56 (4H, m), 8.33-8.40 (2H, m).

後処理

  1. customwas degassed with nitrogen for 30 min
  2. temperaturebefore heating at 50° C. for 18 h
  3. temperatureThe resulting dark suspension was cooled to ambient temperature
  4. stirringstirred at ambient temperature for 4 h
  5. filtrationThe solid was collected by filtration
  6. washwashed with water
  7. customdried under suction

出典と根拠

ORDレコード
ord-e297d0692ae94dd882d2b5ef5e2c80f7
出典データセット
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06617326B2

反応ノート

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