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Acetic Anhydride → N-(5-methyl-1H-pyrazol-3-yl)acetamide

HRID 1953802
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반응식

HRID 1953802 반응식
C(=O)(O)[O-].[Na+].[NH2:6][C:7]1[CH:11]=[C:10]([CH3:12])[NH:9][N:8]=1.[C:13](OC(=O)C)(=[O:15])[CH3:14]>O>[C:13]([NH:6][C:7]1[CH:11]=[C:10]([CH3:12])[NH:9][N:8]=1)(=[O:15])[CH3:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 931461H-Pyrazol-3-amine, 5-methyl-HCID 516892Sodium Bicarbonate

생성물 1

HCID 5246311N-(5-methyl-1H-pyrazol-3-yl)acetamide수율 59.6%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

50.4 g (0.6 mol) of sodium bicarbonate were added in small amounts at room temperature to a solution of 19.4 g (0.2 mol) of 3-amino-5-methyl-1H-pyrazole in 200 cm3 of water. 37.8 cm3 (0.4 mol) of acetic anhydride were added dropwise to this solution and then the mixture was heated at reflux for 2 hours. The solution was subsequently brought back to room temperature, a white solid crystallized and was pulled dry on sintered glass and then washed with 100 cm3 of water. After drying under vacuum at 40° C., 16.6 g of the expected product were obtained in the form of pearlescent-white crystals, the melting point of which was between 210° C. and 212° C.

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후처리

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 2 hours
  3. customwas subsequently brought back to room temperature
  4. customa white solid crystallized
  5. customwas pulled dry on sintered glass
  6. washwashed with 100 cm3 of water
  7. customAfter drying under vacuum at 40° C.

출처 및 근거

ORD 기록
ord-e6217960ed134687af208f44f197710d
출처 데이터셋
uspto-grants-2000_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06118008

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