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Hydrazine hydrate (1:1) → 3-[(2,2,3,3,4,4,4-Heptafluorobutoxy)methyl]aniline

HRID 359607
ノート
印刷プレビュー

反応式

HRID 359607 の反応式
[F:1][C:2]([F:22])([C:15]([F:21])([F:20])[C:16]([F:19])([F:18])[F:17])[CH2:3][O:4][CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([N+:12]([O-])=O)[CH:7]=1.O.NN>C(O)C>[F:1][C:2]([F:22])([C:15]([F:20])([F:21])[C:16]([F:17])([F:18])[F:19])[CH2:3][O:4][CH2:5][C:6]1[CH:7]=[C:8]([CH:9]=[CH:10][CH:11]=1)[NH2:12]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 14330157HCID 14330157、化合物

生成物 1

HCID 150849773-[(2,2,3,3,4,4,4-Heptafluorobutoxy)methyl]aniline

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

180 g (0.54 mol) of 1-(2,2,3,3,4,4,4-heptafluorobutoxy)methyl-3-nitrobenzene (Compound No. 11) obtained in Example 2 was dissolved in 500 ml of ethanol, and the mixture was refluxed for 30 minuted after adding 7.9 g of FeCl3.6H2O and 12.5 g of activated carbon thereto. While the mixture was being stirred, 100 g (2.00 mol) of hydrazine hydrate was added dropwise thereto so as not to cause violent foaming. The mixture was refluxed for 2 hours after the completion of the dropping, thereby completing the reaction. After the reaction mixture was left to cool, the reaction mixture was filtered through a Celite layer and washed with ethanol. The filtrate was concentrated and dissolved in 500 ml of benzene. The solution was successively washed with water and saturated saline solution and was dried by anhydrous sodium sulfate.

後処理

  1. custom11) obtained in Example 2
  2. temperaturethe mixture was refluxed for 30 minuted
  3. temperatureThe mixture was refluxed for 2 hours after the completion of the dropping
  4. customthe reaction
  5. waitAfter the reaction mixture was left
  6. temperatureto cool
  7. filtrationthe reaction mixture was filtered through a Celite layer
  8. washwashed with ethanol
  9. concentrationThe filtrate was concentrated
  10. dissolutiondissolved in 500 ml of benzene
  11. washThe solution was successively washed with water and saturated saline solution
  12. dry with materialwas dried by anhydrous sodium sulfate

出典と根拠

ORDレコード
ord-9ee8363717514038ab07fa4258060416
出典データセット
uspto-grants-1991_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05001275

反応ノート

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