1,2-Dichloroethane → Benzonitrile, 4-(5-heptyl-2-pyrimidinyl)-

HRID 461307ノート

反応式

HRID 461307 の反応式
C([C:8]1[CH:13]=[CH:12][N:11]=[C:10]([C:14]2[CH:22]=[CH:21][C:17]([C:18]([NH2:20])=O)=[CH:16][CH:15]=2)[N:9]=1)CCCCCC.[CH2:23](Cl)[CH2:24]Cl.P(Cl)(Cl)(Cl)=O>CCOCC>[CH2:16]([C:13]1[CH:12]=[N:11][C:10]([C:14]2[CH:15]=[CH:16][C:17]([C:18]#[N:20])=[CH:21][CH:22]=2)=[N:9][CH:8]=1)[CH2:15][CH2:14][CH2:22][CH2:21][CH2:23][CH3:24]

参加物

5

反応物 3

HCID 111,2-DichloroethaneHCID 24813Phosphorus oxychlorideHCID 538442864-(4-n-Heptylpyrimid-2-yl)benzoic acid amide

生成物 1

HCID 108846Benzonitrile, 4-(5-heptyl-2-pyrimidinyl)-

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

1.9 g. of 4-(4-n-heptylpyrimid-2-yl)benzoic acid amide are left for 80 minutes under reflux in a mixture of 40 ml. of ethylene chloride and 0.63 ml. of phosphorus oxychloride, with stirring. The reaction mixture, diluted with ether, is washed with 2N sodium hydroxide solution and then with water until neutral. After evaporation of the organic phase, drying over sodium sulfate, 1.9 g. of 5-n-heptyl-2-(4-cyanophenyl)-pyrimidine result, which are distilled in a high vacuum, having a m.p. of 44.2°-44.7°; cl.p. 50.1°-50.4°.

後処理

  1. temperatureunder reflux in a mixture of 40 ml
  2. washis washed with 2N sodium hydroxide solution
  3. customAfter evaporation of the organic phase
  4. dry with materialdrying over sodium sulfate, 1.9 g

出典と根拠

ORDレコード
ord-aa5edd4b8d9c45928ad767ebc30ae839
出典データセット
uspto-grants-1977_12
特許番号
US04062798

反応ノート

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