Hydrochloric Acid → HCID 19802057、化合物
反応式
[OH:1][CH:2]([CH2:6][O:7][S:8]([CH3:11])(=[O:10])=[O:9])[CH2:3][C:4]#[N:5].[ClH:12].[H][H]>CO.[Pd]>[ClH:12].[OH:1][CH:2]([CH2:6][O:7][S:8]([CH3:11])(=[O:10])=[O:9])[CH2:3][CH2:4][NH2:5]参加物
6
実験手順
To a solution of (RS)-3-hydroxy-4-(methanesulfonyloxy)butyronitrile (14.6 g) in methanol (60 ml), 10 wt. % Pd on carbon (2.5 g) and conc. hydrochloric acid (15 ml) were added. The mixture was stirred in a hydrogen atmosphere of 4.0 kg/cm2 at room temperature for 8 hours. After filtering off the catalyst, the mixture was evaporated under reduced pressure to obtain a crude product, which was purified by silica gel chromatography (Wako Gel C200, an eluent: methanol/acetone (volume ratio of 1/9) to obtain pure (RS)-3-hydroxy-4-(methanesulfonyloxy)butylamine hydrochloride (15.4 g). Yield, 85 %.
後処理
- filtrationAfter filtering off the catalyst
- customthe mixture was evaporated under reduced pressure
- customto obtain a crude product, which
- customwas purified by silica gel chromatography (Wako Gel C200
出典と根拠
- ORDレコード
- ord-62f4fe002bd94cd78cdcaf8644865748
- 出典データセット
- uspto-grants-1993_01
- 特許番号
- US05179212
反応ノート
読み込み中…