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Hydrazine hydrate (1:1) → HCID 178506330、化合物

HRID 1983039
ノート
印刷プレビュー

反応式

HRID 1983039 の反応式
O.[NH2:2]N.[F:4][C:5]([F:15])([C:11]([F:14])([F:13])[F:12])[C:6](OCC)=O.C(O)(=O)C.[CH:20]([NH2:22])=[NH:21]>C(O)C>[F:4][C:5]([F:15])([C:6]1[N:22]=[CH:20][NH:21][N:2]=1)[C:11]([F:14])([F:13])[F:12]
参加物反応条件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 24654Hydrazine hydrate (1:1)HCID 67928Propanoic acid, 2,2,3,3,3-pentafluoro-, ethyl esterHCID 160693Formamidine acetate

生成物 1

HCID 178506330HCID 178506330、化合物収率 63.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
0 °C

実験手順

1.25 g of hydrazine hydrate was dissolved to 45 ml of ethanol, and it was cooled to 0° C. 5.38 g of ethyl 2,2,3,3,3-pentafluoropropionate was dropped to it over the period of 15 minutes, followed by stirring at 0° C. for 1 hour. 2.61 g of formamidine acetic acid salt was added to the reaction mixture, followed by stirring at room temperature for 30 minutes. The reaction mixture was concentrated under reduced pressure. 50 ml of acetic acid was added to the residue, followed by stirring at 100° C. for 5 hours. The reaction mixture was concentrated under reduced pressure. Saturated aqueous solution of sodium hydrogen carbonate was added to the residue so as to be around pH 6. And then it was extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 2.98 g of 3-pentafluoroethyl-1H-1,2,4-triazole.

後処理

  1. stirringby stirring at room temperature for 30 minutes
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. addition50 ml of acetic acid was added to the residue
  4. stirringby stirring at 100° C. for 5 hours
  5. concentrationThe reaction mixture was concentrated under reduced pressure
  6. additionSaturated aqueous solution of sodium hydrogen carbonate was added to the residue so as
  7. extractionAnd then it was extracted with ethyl acetate
  8. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  9. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-d3e78bbd11e245cfae2d386e9301bac4
出典データセット
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07541374B2

反応ノート

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