Formic Acid → 5-Formamido-1-methylpyrazole

HRID 1088042노트

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HRID 1088042 반응식
C(O[C:5](=[O:7])C)(=O)C.C(O)=O.[NH2:11][C:12]1[N:16]([CH3:17])[N:15]=[CH:14][CH:13]=1.C(=O)([O-])[O-].[K+].[K+]>C(OCC)(=O)C.O>[CH:5]([NH:11][C:12]1[N:16]([CH3:17])[N:15]=[CH:14][CH:13]=1)=[O:7]

참가 물질

7

반응물 4

HCID 284Formic AcidHCID 7918Acetic AnhydrideHCID 11430Potassium CarbonateHCID 1369272-Methyl-2H-pyrazol-3-ylamine

생성물 1

HCID 27558695-Formamido-1-methylpyrazole

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

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온도
45 °C

실험 절차

A mixture of acetic anhydride (38.86 ml) and formic acid (15.54 ml) was stirred at 45° C. for 45 minutes. To this mixture was added 5-amino-1-methylpyrazole (10 g) under ice-cooling, and the reaction mixture was stirred at the same temperature for 10 minutes. The resultant mixture was poured into a mixture of water and ethyl acetate, and the resultant solution was adjusted to pH 8 with potassium carbonate. The organic layer was separated, and the aqueous layer was extracted with ethyl acetate six times. The organic layers were combined, dried over magnesium sulfate, and evaporated in vacuo to give 5-formamido-1-methylpyrazole (12.88 g).

후처리

  1. temperaturecooling
  2. stirringthe reaction mixture was stirred at the same temperature for 10 minutes
  3. customThe organic layer was separated
  4. extractionthe aqueous layer was extracted with ethyl acetate six times
  5. dry with materialdried over magnesium sulfate
  6. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-9206a6f7eee346e58dfea350bde7b11e
출처 데이터셋
uspto-grants-1990_10
특허 번호
US04960766

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