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Methanol → 1-(4'-Chloro-4-nitro-biphen-2-yl)-ethanone

HRID 1788583
ノート
印刷プレビュー

反応式

HRID 1788583 の反応式
Br[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[C:11](=[O:13])[CH3:12].[Cl:14][C:15]1[CH:20]=[CH:19][C:18](B(O)O)=[CH:17][CH:16]=1.CO.C(=O)(O)[O-].[Na+]>C1(C)C=CC=CC=1.[Pd].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[Cl:14][C:15]1[CH:20]=[CH:19][C:18]([C:2]2[C:3]([C:11](=[O:13])[CH3:12])=[CH:4][C:5]([N+:8]([O-:10])=[O:9])=[CH:6][CH:7]=2)=[CH:17][CH:16]=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

7

反応物 4

HCID 887MethanolHCID 742994-Chlorophenylboronic acidHCID 516892Sodium BicarbonateHCID 234021201-(2-Bromo-5-nitrophenyl)ethanone

生成物 1

HCID 860270631-(4'-Chloro-4-nitro-biphen-2-yl)-ethanone

試薬・触媒・溶媒 2

HCID 11979704
Tetrakis(triphenylphosphine)palladium
触媒
HCID 1140Toluene溶媒

反応条件

温度
80 °C

実験手順

1-(2-Bromo-5-nitro-phenyl)-ethanone (1 g, 4 mmol; prepared similarly to the procedure described in Meisenheimer, J., Zimmermann P., and v. Kummer, U. Ann. der. Chem. 446, pp. 205-228), p-Chlorophenylboronic acid (768 mg, 1.2 eq.), and tetrakis(triphenylphosphine)-palladium(0) (473 mg, 0.1 eq.), were dissolved in 25 mL toluene, 6 mL methanol and 2.5 mL sat. sodium bicarbonate solution. After degassing/sonicating the solution, the sealed reaction vessel was heated to 80° C. overnight. The cooled solution was separated between ethyl acetate and water; the aqueous phase extracted two more times with ethyl acetate, and the organic fractions were combined, dried with sodium sulfate and evaporated. Silica gel chromatography (4:1 hexanes/ethyl acetate) gave 1-(4′-chloro-4-nitro-biphen-2-yl)-ethanone (962 mg).

後処理

  1. customprepared similarly to the procedure
  2. customAfter degassing/sonicating the solution
  3. customthe sealed reaction vessel
  4. customThe cooled solution was separated between ethyl acetate and water
  5. extractionthe aqueous phase extracted two more times with ethyl acetate
  6. dry with materialdried with sodium sulfate
  7. customevaporated

出典と根拠

ORDレコード
ord-db6a3b04c04d45caaa23c9fa24f0ced6
出典データセット
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07511145B2

反応ノート

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