Acetic Anhydride → HCID 178474341、化合物

HRID 38672ノート

反応式

HRID 38672 の反応式
[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

参加物

5

反応物 3

HCID 7918Acetic AnhydrideHCID 516892Sodium BicarbonateHCID 178418806HCID 178418806、化合物

生成物 1

HCID 178474341HCID 178474341、化合物収率 49.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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+).

後処理

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

出典と根拠

ORDレコード
ord-2e273e05783d458eb9aeaf2f9b579303
出典データセット
uspto-grants-2013_09
特許番号
US08524750B2

反応ノート

読み込み中…