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Pyridine → 4-Fluorobenzamide

HRID 1826704
ノート
印刷プレビュー

反応式

HRID 1826704 の反応式
[N:1]1C=CC=C(OC2C=C(C=C(C#N)C=2)N)C=1.N1C=CC=CC=1.[F:23][C:24]1[CH:32]=[CH:31][C:27]([C:28](Cl)=[O:29])=[CH:26][CH:25]=1>C(Cl)Cl>[F:23][C:24]1[CH:32]=[CH:31][C:27]([C:28]([NH2:1])=[O:29])=[CH:26][CH:25]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1049PyridineHCID 678794-Fluorobenzoyl chlorideHCID 22136195HCID 22136195、化合物

生成物 1

HCID 715724-Fluorobenzamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

Formula I where R1 is Pyridin-3-yl, R2 is CN, and R3 is 4-Fluorophenyl To a solution of 1 eq. ( 0.1 g, 0.473 mmol) of 3-(pyridin-3-yloxy)-5-cyano-aniline in 0.47 M in CH2Cl2 (1 mL) and 1.6 eq. of pyridine (0.56 g, 0.71 mmol) was added 3 eq. of 4-fluorobenzoyl chloride (0.225 g, 1.42 mmol) and the resultant mixture stirred at rt overnight. The reaction mixture was diluted with CH2Cl2, washed with sat. NaHCO3, dried (Na2SO4) and concentrated in vacuo. The resultant residue was diluted with toluene and concentrated in vacuo (5 times). Purification by chromatography over silica with 5% MeOH/CH2Cl2 as the eluant afforded 134 mg of a the desired title compound of Formula I, N-[3-cyano-5-(pyridin-3-yloxy)-phenyl]]-4-fluoro-benzamide, as a solid (85% yield). Mpt 169–172° C. MS (M−1) 332.3.

後処理

  1. washwashed with sat. NaHCO3
  2. dry with materialdried (Na2SO4)
  3. concentrationconcentrated in vacuo
  4. additionThe resultant residue was diluted with toluene
  5. concentrationconcentrated in vacuo (5 times)
  6. customPurification by chromatography over silica with 5% MeOH/CH2Cl2 as the eluant

出典と根拠

ORDレコード
ord-2f7169e922ee42b19bd21418c16f21db
出典データセット
uspto-grants-2006_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07053094B2

反応ノート

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