Hydrochloric Acid → 4-Hydroxy-1,3,3-trimethyl-3,4-dihydroquinolin-2(1H)-one
反応式
[BH4-].[Na+].[CH3:3][N:4]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[C:7](=[O:14])[C:6]([CH3:16])([CH3:15])[C:5]1=[O:17].Cl>CCO>[OH:14][CH:7]1[C:8]2[C:13](=[CH:12][CH:11]=[CH:10][CH:9]=2)[N:4]([CH3:3])[C:5](=[O:17])[C:6]1([CH3:16])[CH3:15]参加物
5
実験手順
NaBH4 (excess amount) is added to a solution of 1,3,3-Trimethyl-1H-quinoline-2,4-dione (330 mg, 1.62 mmol) in EtOH (8 mL) at 0° C. The resulting mixture is slowly warmed up to room temperature. After 1 h, HCl (10%, 3 mL) is added dropwise. The solvent is removed under vacuum, the residue is dissolved into ether and washed with water, brine, and dried over anhydrous Na2SO4. After concentration, the title compound is yielded (275 mg, 82% yield).
後処理
- customThe solvent is removed under vacuum
- dissolutionthe residue is dissolved into ether
- washwashed with water, brine
- dry with materialdried over anhydrous Na2SO4
- concentrationAfter concentration
出典と根拠
- ORDレコード
- ord-c63cda62eac443e8bccd8558c3f3c63a
- 出典データセット
- uspto-grants-2012_03
- 特許番号
- US08143278B2
反応ノート
読み込み中…