Hydrochloric Acid → (E)-4-(cyclobutyl(methyl)amino)but-2-enoic acid hydrochloride
反応式
[CH:1]1([N:5]([CH3:13])[CH2:6]/[CH:7]=[CH:8]/[C:9]([O:11]C)=[O:10])[CH2:4][CH2:3][CH2:2]1.O[Li].O.[ClH:17]>C1COCC1.O>[ClH:17].[CH:1]1([N:5]([CH3:13])[CH2:6]/[CH:7]=[CH:8]/[C:9]([OH:11])=[O:10])[CH2:2][CH2:3][CH2:4]1参加物
5
実験手順
To a solution of (E)-methyl 4-(cyclobutyl(methyl)amino)but-2-enoate (20) (1.47 g, 8 mmol) in THF/H2O (8 mL/2 mL) was added LiOH.H2O (730 mg, 16 mmol). The reaction mixture was stirred at RT overnight, then acidified with 1N HCl to pH=1 and concentrated in vacuum to afford (E)-4-(cyclobutyl(methyl)amino)but-2-enoic acid hydrochloride salt (21) (2.31 g, 97%, mixed with LiCl) as a white solid which was used in the next step without purification. LC-MS (ESI): m/z (M+1) 170.2.
後処理
- concentrationconcentrated in vacuum
出典と根拠
- ORDレコード
- ord-efee41ebc1db4ab0989bc7b232a3cb47
- 出典データセット
- uspto-grants-2013_02
- 特許番号
- US08377946B1
反応ノート
読み込み中…