Lithium Hydroxide → N-(2-fluoroethyl)-N-methyloxamic acid
反応式
[F:1][CH2:2][CH2:3][N:4]([CH3:12])[C:5](=[O:11])[C:6]([O:8]CC)=[O:7].[Li+].[OH-]>CO.O>[F:1][CH2:2][CH2:3][N:4]([CH3:12])[C:5](=[O:11])[C:6]([OH:8])=[O:7]参加物
4
実験手順
To a solution of ethyl 2-((2-fluoroethyl)(methyl)amino)-2-oxoacetate (1.2 g, 7.36 mmol) in methanol/water (30 mL, 1:1) was added LiOH (0.352 g, 14.71 mmol). The solution was stirred for 2 h. The methanol was removed by concentration and concentrated HCl (2 mL) was added. The solvent was removed and the residue dissolved in CH2Cl2 and filtered. The filtrate was concentrated to give the title compound as an off-white crystalline powder (0.615 g, 56% yield). 1H NMR (400 MHz, CDCl3) δ: 4.47-4.89 (2 H, m) 3.67-4.39 (2 H, m) 3.07-3.60 (3 H, m).
後処理
- customThe methanol was removed by concentration and concentrated HCl (2 mL)
- additionwas added
- customThe solvent was removed
- dissolutionthe residue dissolved in CH2Cl2
- filtrationfiltered
- concentrationThe filtrate was concentrated
出典と根拠
- ORDレコード
- ord-e959f6e3c945458ea2af07eda1ca0a8e
- 出典データセット
- uspto-grants-2012_03
- 特許番号
- US08129398B2
反応ノート
読み込み中…