Acetic Anhydride → HCID 178474341、化合物

HRID 32793ノート

反応式

HRID 32793 の反応式
[NH2:1][C:2]1[CH:6]=[CH:5][NH:4][N:3]=1.C([O-])(O)=O.[Na+].[CH3:12][C:13](OC(C)=O)=[O:14]>O>[NH:4]1[CH:5]=[CH:6][C:2]([NH:1][C:13](=[O:14])[CH3:12])=[N:3]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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a solution of 3-aminopyrazole (20 g, 0.24 mol) in H2O (36 mL), at 5-10° C., was slowly added NaHCO3 (9.1 g, mol, 3 eq) and then Ac2O (6.79 ml, 2 eq). The reaction mixture was refluxed for 8 hr. It was cooled down to r.t. and was left standing at this temperature for 12 hr to allow crystallization. The white solid was filtered (12.9 g) and the mother liquor volume was reduced. A second batch of white solid (3.4 g) was obtained after crystallization. The two batches were combined to give the title compound (16.3 g, 54%).

後処理

  1. customat 5-10° C.
  2. temperatureThe reaction mixture was refluxed for 8 hr
  3. waitwas left
  4. customcrystallization
  5. filtrationThe white solid was filtered (12.9 g)

出典と根拠

ORDレコード
ord-d8cc33e5f25f40949a2c7f8221c44612
出典データセット
uspto-grants-2008_09
特許番号
US07427630B2

反応ノート

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