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Formic Acid → HCID 15580713、化合物

HRID 543807
ノート
印刷プレビュー

反応式

HRID 543807 の反応式
[CH:1](O)=O.Cl[C:5]1[CH:6]=[C:7]([N:12]2[CH2:16][CH:15](C)[C:14]([NH:18][CH:19]=[O:20])=[N:13]2)[CH:8]=[CH:9][C:10]=1[Cl:11].CCCCCC>ClCCl>[Cl:11][C:10]1[CH:5]=[CH:6][C:7]([N:12]2[CH:16]([CH3:1])[CH2:15][C:14]([NH:18][CH:19]=[O:20])=[N:13]2)=[CH:8][CH:9]=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 284Formic AcidHCID 8058HexaneHCID 15580721HCID 15580721、化合物

生成物 1

HCID 15580713HCID 15580713、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A 4.8 g. amount of the above compound is dissolved in 25.0 ml. of a mixture of formic acid and acetic anhydride (Example 15). The reaction mixture is allowed to remain at room temperature for 3 hours, then ice water is added to separate a gum. The aqueous phase is decanted and the gum is dissolved in dichloromethane. The solution is dried over magnesium sulfate and passed through a hydrous magnesium silicate. The effluent is evaporated leaving a gum. The gum is dissolved in dichloromethane. The solution is heated and hexane is added until turbidity results. The mixture is cooled and filtered to yield 3.6 g. of the desired product as off-white crystals, m.p. 112°-113° C.

後処理

  1. dissolutionamount of the above compound is dissolved in 25.0 ml
  2. customto separate a gum
  3. customThe aqueous phase is decanted
  4. dissolutionthe gum is dissolved in dichloromethane
  5. dry with materialThe solution is dried over magnesium sulfate
  6. customThe effluent is evaporated
  7. customleaving a gum
  8. temperatureThe solution is heated
  9. customresults
  10. temperatureThe mixture is cooled
  11. filtrationfiltered
  12. customto yield 3.6 g

出典と根拠

ORDレコード
ord-7dfb4421598d4434b20f29083858d976
出典データセット
uspto-grants-1984_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04447442

反応ノート

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