Hydrochloric Acid → Methyl 3-amino-2-(aminomethyl)propanoate--hydrogen chloride (1/2)
反応式
[Na].[C:2]([CH:4]([C:9]#[N:10])[C:5]([O:7][CH3:8])=[O:6])#[N:3].[ClH:11]>[Pd].CO>[ClH:11].[ClH:11].[NH2:3][CH2:2][CH:4]([CH2:9][NH2:10])[C:5]([O:7][CH3:8])=[O:6]参加物
6
実験手順
A stirring suspension of 10% palladium on carbon (2.0 g) in a solution of the sodium salt of methyl dicyanoacetate (1.00 g, 6.20 mmol) in methanol (100 mL) containing concd hydrochloric acid (32%, 2.0 mL) was hydrogenated at 5 bar and rt. for 24 h. The catalyst was removed by filtration and the solvent was evaporated in vacuo. The residue was treated with methanol (50 mL) and the precipitated sodium chloride was removed by filtration. The solution was concentrated to a low volume in vacuo and then EtOAc was added to precipitate the bis-hydrochloride 12 as an off-white solid (1.20 g).
後処理
- customwas hydrogenated at 5 bar and rt
- customThe catalyst was removed by filtration
- customthe solvent was evaporated in vacuo
- additionThe residue was treated with methanol (50 mL)
- customthe precipitated sodium chloride was removed by filtration
- concentrationThe solution was concentrated to a low volume in vacuo
- additionEtOAc was added
- customto precipitate the bis-hydrochloride 12 as an off-white solid (1.20 g)
出典と根拠
- ORDレコード
- ord-d34920a17b1f477aa587b03d527648c2
- 出典データセット
- uspto-grants-2010_07
- 特許番号
- US07759519B2
反応ノート
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