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Potassium Carbonate → HCID 13362794、化合物

HRID 365059
ノート
印刷プレビュー

反応式

HRID 365059 の反応式
[C:1]([C:3]1[CH:16]=[CH:15][C:6]([O:7][C:8]2[CH:13]=[CH:12][C:11]([OH:14])=[CH:10][CH:9]=2)=[CH:5][CH:4]=1)#[N:2].Br[CH:18]([CH3:28])[C:19]([NH:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)=[O:20].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[C:22]1([NH:21][C:19](=[O:20])[CH:18]([O:14][C:11]2[CH:12]=[CH:13][C:8]([O:7][C:6]3[CH:15]=[CH:16][C:3]([C:1]#[N:2])=[CH:4][CH:5]=3)=[CH:9][CH:10]=2)[CH3:28])[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=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 11430Potassium CarbonateHCID 991132-Bromo-N-phenylpropionamideHCID 45227124-(4-Hydroxyphenoxy)benzonitrile

生成物 1

HCID 13362794HCID 13362794、化合物収率 68.8%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To 30 ml of acetone were added 1.06 g of 4-(4-cyanophenoxy)-phenol, 0.99 g of α-bromopropionanilide and 0.83 g of anhydrous potassium carbonate, and the mixture wask subjected to reflux for 16 hours with stirring. After the reaction mixture was cooled and separated from inorganic salts through filtration, acetone was distilled away therefrom. The residue was purified through a column-chromatography [silica gel, developed with ethyl acetate/n-hexane=1/1(V/V)] to give 1.07 g of the title compound (yield 60%), which was recrystallized from a mixed solvent of benzene-n-hexane to afford a crystal of melting point 133°-134° C.

後処理

  1. temperatureto reflux for 16 hours
  2. temperatureAfter the reaction mixture was cooled
  3. customseparated from inorganic salts through filtration, acetone
  4. distillationwas distilled away
  5. customThe residue was purified through a column-chromatography [silica gel

出典と根拠

ORDレコード
ord-69b212377b6e44eb8aa82304a4803d6a
出典データセット
uspto-grants-1986_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04608081

反応ノート

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