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Triethylamine → HCID 178518989、化合物

HRID 375064
ノート
印刷プレビュー

反応式

HRID 375064 の反応式
C(N1C=CN=C1)(N1C=CN=C1)=O.C(N(CC)CC)C.[Cl:20][C:21]1[CH:22]=[C:23]([OH:31])[C:24](=[CH:29][CH:30]=1)[C:25]([NH:27]O)=[O:26]>O1CCCC1>[Cl:20][C:21]1[CH:30]=[CH:29][C:24]2[C:25]([OH:26])=[N:27][O:31][C:23]=2[CH:22]=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 8471TriethylamineHCID 682631,1'-CarbonyldiimidazoleHCID 27818484-chloro-N,2-dihydroxybenzamide

生成物 1

HCID 178518989HCID 178518989、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 1,1'-carbonyldiimidazole (12.76 g, 78.5 mmol) and triethylamine (12.6 mL, 90 mmol) in tetrahydrofuran is slowly added to a refluxing suspension of 4-chlorosalicylohydroxamic acid (13.39 g, 71.4 mmol) in tetrahydrofuran. The reaction mixture is refluxed for 1 hour, cooled, concentrated in vacuo, diluted with water, acidified with concentrated hydrochloric acid (pH1) and filtered to obtain a solid. A solution of the solid in ether is extracted with saturated sodium hydrogen carbonate solution. The combined aqueous extracts are acidified with concentrated hydrochloric acid and the resultant precipitate is collected and dried overnight to give the title product as a white solid, mp 218°-219° C.

後処理

  1. temperatureThe reaction mixture is refluxed for 1 hour
  2. temperaturecooled
  3. concentrationconcentrated in vacuo
  4. additiondiluted with water
  5. filtrationfiltered
  6. customto obtain a solid
  7. extractionA solution of the solid in ether is extracted with saturated sodium hydrogen carbonate solution
  8. customthe resultant precipitate is collected
  9. customdried overnight

出典と根拠

ORDレコード
ord-b852751fee0647c097c48f4f1949f9f2
出典データセット
uspto-grants-1996_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05484763

反応ノート

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