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

반응식

[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]

참가 물질

반응물 2

HCID 7918Acetic Anhydride

HCID 92211H-Indazole

생성물 1

HCID 159392751-(2H-Indazol-2-yl)ethanone수율 96%

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록: ord-ac4aa83f38ff4124a7a94ff493f1d086
출처 데이터셋: uspto-grants-2005_02
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US06849649B2

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