Acetic Anhydride → HCID 178474341, 화합물

HRID 38672노트

반응식

HRID 38672 반응식
[NH:1]1[CH:5]=[CH:4][C:3]([NH2:6])=[N:2]1.C([O-])(O)=O.[Na+].[C:12](OC(=O)C)(=[O:14])[CH3:13]>O>[NH:1]1[CH:5]=[CH:4][C:3]([NH:6][C:12](=[O:14])[CH3:13])=[N:2]1

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 516892Sodium BicarbonateHCID 178418806HCID 178418806, 화합물

생성물 1

HCID 178474341HCID 178474341, 화합물수율 49.3%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

1H-pyrazol-3-amine (ALDRICH, 11.32 g, 0.136 mol) was dissolved in 100 mL of distilled water. NaHCO3 (34 g, 0.408 mol) was slowly added. Acetic anhydride (27.55 g, 0.272 mol) was then added dropwise and the resulting suspension was heated at reflux overnight. Then, the mixture was allowed to cool down to r.t. and the solid obtained was filtered off and characterized as the title compound (8.4 g, 0.067 mol, 49%). After concentration of the filtrate, a second precipitate was obtained (2.7 g, 0.021 mol, 16%), also characterized as the title compound. 1H NMR (300 MHz, DMSO-d6) δ ppm: 12.23 (br s, 1H), 10.30 (br s, 1H), 7.55 (br s, 1H), 6.45 (br s, 1H), 1.97 (s, 3H). [ES+MS] m/z 126 (MH+).

후처리

  1. temperaturethe resulting suspension was heated
  2. temperatureat reflux overnight
  3. customthe solid obtained
  4. filtrationwas filtered off

출처 및 근거

ORD 기록
ord-2e273e05783d458eb9aeaf2f9b579303
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08524750B2

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