Hydrochloric Acid → (2-Methyl-but-3-enyloxy)-acetic acid
反応式
[CH3:1][CH:2]([CH:5]=[CH2:6])[CH2:3][OH:4].[H-].[Na+].[C:9]([O:12]I)(=[O:11])[CH3:10].[Na].Cl>C1COCC1.O.[Cl-].[Na+].O>[CH3:1][CH:2]([CH:5]=[CH2:6])[CH2:3][O:4][CH2:10][C:9]([OH:12])=[O:11]参加物
8
実験手順
Under nitrogen atmosphere a suspension of 0.5 g (5.81 mmol) 2-methyl-3-buten-1-ol and 0.348 g (8.71 mmol, 60% suspension in mineral oil) NaH in 10 ml THF are stirred 3 h at rt. Solid sodium iodo acetate (1.81 g, 8.71 mmol) is added and stirring is continued for 2 h. The mixture is diluted with water and brine, acidified with 1N HCl and extracted with EtOAc. The organic phase is dried with sodium sulfate and concentrated. the residue is kugelrohr distilled at ca 1 mbar (70-110° C.) to yield the title compound as a colorless liquid.
後処理
- stirringstirring
- waitis continued for 2 h
- extractionextracted with EtOAc
- dry with materialThe organic phase is dried with sodium sulfate
- concentrationconcentrated
- distillationthe residue is kugelrohr distilled at ca 1 mbar (70-110° C.)
出典と根拠
- ORDレコード
- ord-35c6ff1aa2b94935a9f8a0cf1453e540
- 出典データセット
- uspto-grants-2009_11
- 特許番号
- US07612055B2
反応ノート
読み込み中…
