Acetyl chloride → (S)-N-(1-(5-Hydroxypyridin-2-yl)ethyl)acetamide
反応式
[NH2:1][C@H:2]([C:4]1[N:9]=[CH:8][C:7]([OH:10])=[CH:6][CH:5]=1)[CH3:3].[C:11](Cl)(=[O:13])[CH3:12]>C1COCC1>[OH:10][C:7]1[CH:6]=[CH:5][C:4]([C@@H:2]([NH:1][C:11](=[O:13])[CH3:12])[CH3:3])=[N:9][CH:8]=1参加物
4
実験手順
To 1.00 g (5.73 mmol) (S)-6-(1-aminoethyl)pyridin-3-ol in 10 ml THF and 3.99 mL TEA (28.6 mmol) are slowly added 494 mg (6.30 mmol) acetyl chloride and stirring is continued for 2 h. The reaction is quenched by the addition of water and extracted several times with DCM. The org. layers are combined, dried over MgSO4, filtered and the solvent is removed in vacuo. The crude product is purified by column chromatography (silica gel, DCM/MeOH/NH3 90/9/1).
後処理
- customThe reaction is quenched by the addition of water
- extractionextracted several times with DCM
- dry with materialdried over MgSO4
- filtrationfiltered
- customthe solvent is removed in vacuo
- customThe crude product is purified by column chromatography (silica gel, DCM/MeOH/NH3 90/9/1)
出典と根拠
- ORDレコード
- ord-e05a20423a9346b1b6c342b34195757b
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08530460B2
反応ノート
読み込み中…