Diethyl (ethoxymethylene)malonate → HCID 178469698、化合物

HRID 477543ノート

反応式

HRID 477543 の反応式
[NH2:1][C:2]1[N:6]=[C:5]([SH:7])[NH:4][N:3]=1.C([O:10][CH:11]=[C:12]([C:18](OCC)=O)[C:13]([O:15][CH2:16][CH3:17])=[O:14])C>C(O)(=O)C>[CH2:16]([O:15][C:13]([C:12]1[CH:18]=[N:1][C:2]2[N:3]([N:4]=[C:5]([SH:7])[N:6]=2)[C:11]=1[OH:10])=[O:14])[CH3:17]

参加物

4

反応物 2

HCID 6871Diethyl (ethoxymethylene)malonateHCID 1785092965-amino-1H-1,2,4-triazole-3-thiol

生成物 1

HCID 178469698HCID 178469698、化合物収率 29%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture of 15 g 3-amino-5-mercapto-s-triazole, 28 g diethyl ethoxymethylenemalonate and 70 ml acetic acid was refluxed for 18 hours. After removing the solvent by distillation, the remaining brown oil was allowed to cool to room temperature, and the pH was adjusted to 10 with sodium hydroxide solution. After washing with 100 ml ethyl acetate, the brown aqueous solution was neutralized to pH 7.5 with 6N hydrochloric acid, and again washed with 100 ml ethyl acetate. The pH of the aqueous layer was lowered to 3.0 with 6N hydrochloric acid, and the separated crude product (12 g) was collected by filtration and recrystallized from 30 ml methanol, giving 9 g of the objective compound as colorless crystals.

後処理

  1. temperaturewas refluxed for 18 hours
  2. customAfter removing the solvent
  3. distillationby distillation
  4. washAfter washing with 100 ml ethyl acetate
  5. washagain washed with 100 ml ethyl acetate
  6. customthe separated crude product (12 g)
  7. filtrationwas collected by filtration
  8. customrecrystallized from 30 ml methanol

出典と根拠

ORDレコード
ord-2f85c0296166417e90a47722439d8cce
出典データセット
uspto-grants-1989_12
特許番号
US04888332

反応ノート

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