Hydrochloric Acid → 2-Amino-4,4-difluorobutanoic acid hydrochloride
反応式
C([O:3][C:4](=[O:19])[C:5]([NH:15]C(=O)C)([CH2:11][CH:12]([F:14])[F:13])C(OCC)=O)C.[ClH:20]>>[ClH:20].[NH2:15][CH:5]([CH2:11][CH:12]([F:14])[F:13])[C:4]([OH:19])=[O:3]参加物
3
実験手順
In a flask was placed 2-acetylamino-2-(2,2-difluoro-ethyl)-malonic acid diethyl ester (8.94 g, 31.78 mmol) and 6N aqueous hydrochloric acid (140 mL). This mixture was refluxed overnight. After this time, the mixture was cooled to room temperature and extracted with diethyl ether (100 mL) the aqueous layer was concentrated in vacuo, azeotroped with acetonitrile and dried under high vacuum to afford 2-amino-4,4-difluoro-butyric acid hydrochloride salt (5.39 g, 97%) as a cream colored solid.
後処理
- customIn a flask was placed
- temperatureThis mixture was refluxed overnight
- extractionextracted with diethyl ether (100 mL) the aqueous layer
- concentrationwas concentrated in vacuo
- customazeotroped with acetonitrile
- customdried under high vacuum
出典と根拠
- ORDレコード
- ord-c9fda19b50b74a45a68557364533658c
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07741327B2
反応ノート
読み込み中…