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Hydrazine hydrate (1:1) → HCID 178506330, 화합물

HRID 1983039
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HRID 1983039 반응식
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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24654Hydrazine hydrate (1:1)HCID 67928Propanoic acid, 2,2,3,3,3-pentafluoro-, ethyl esterHCID 160693Formamidine acetate

생성물 1

HCID 178506330HCID 178506330, 화합물수율 63.8%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d3e78bbd11e245cfae2d386e9301bac4
출처 데이터셋
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07541374B2

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