Acetic Anhydride → HCID 178488021、化合物

反応式

[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[N+:9]([O-])=[CH:8][CH:7]=[CH:6]2.CC(OC(C)=O)=[O:16]>>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[N:9]=[C:8]([OH:16])[CH:7]=[CH:6]2

参加物

反応物 2

HCID 7918Acetic Anhydride

HCID 2538216-Methoxyquinoline N-oxide

生成物 1

HCID 178488021HCID 178488021、化合物収率 67%

実験手順

A solution of 6-methoxyquinoline 1-oxide (300 mg, 1.71 mmol) in Ac2O (5.0 mL) was refluxed for 2 hours. The solvent was removed under reduced pressure. The residue was dissolved in EtOAc (50 mL), the organic layer was washed with brine (10 mL), dried over Na2SO4, filtered and concentrated to give the crude product which was purified by silica gel column (PE/EtOAc=1/2) to give 6-methoxyquinolin-2-ol (200 mg, yield 67%).

後処理

customThe solvent was removed under reduced pressure
dissolutionThe residue was dissolved in EtOAc (50 mL)
washthe organic layer was washed with brine (10 mL)
dry with materialdried over Na2SO4
filtrationfiltered
concentrationconcentrated
customto give the crude product which
customwas purified by silica gel column (PE/EtOAc=1/2)

出典と根拠

ORDレコード: ord-751dab47e7904e4eb8780f4e57067d9c
出典データセット: uspto-grants-2016_09
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US09433618B2

反応ノート

読み込み中…

参加物