Acetic Anhydride → 1-(2H-Indazol-2-yl)ethanone

HRID 431776

反応式

HRID 431776 の反応式
[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH:3]=[N:2]1.[C:10](OC(=O)C)(=[O:12])[CH3:11]>>[C:10]([N:2]1[CH:3]=[C:4]2[C:9]([CH:8]=[CH:7][CH:6]=[CH:5]2)=[N:1]1)(=[O:12])[CH3:11]

参加物

3

反応物 2

HCID 7918Acetic AnhydrideHCID 92211H-Indazole

生成物 1

HCID 159392751-(2H-Indazol-2-yl)ethanone収率 96%

実験手順

Indazole (3.5 g, 29.6 mmol) and acetic anhydride (35 ml) were heated at 60° C. under nitrogen for 3 h. Excess acetic anhydride was evaporated and the remaining oily residue partitioned between 3% aqueous NaHCO3 (20 ml) and EtOAc (30 ml). The organic layer was separated, dried (MgSO4) and evaporated to provide the title product (4.5 g, 96%); 1HNMR (400 MHz, CDCl3) δ: 2.80 (s, 3H), 7.37 (t, 1H), 7.58 (t, 1H), 7.75 (d, 1H), 8.46 (d, 1H).

後処理

  1. customExcess acetic anhydride was evaporated
  2. customthe remaining oily residue partitioned between 3% aqueous NaHCO3 (20 ml) and EtOAc (30 ml)
  3. customThe organic layer was separated
  4. dry with materialdried (MgSO4)
  5. customevaporated

出典と根拠

ORDレコード
ord-e124a37c007a42e380d9c194ec1e6259
出典データセット
uspto-grants-2003_12
特許番号
US06660756B2

関連ノート

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