Hydrochloric Acid → Ethyl indoline-2-carboxylate
反応式
[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH2:3][C@H:2]1[C:10]([OH:12])=[O:11].[ClH:13].[CH2:14](O)[CH3:15]>>[ClH:13].[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH2:3][C@H:2]1[C:10]([O:12][CH2:14][CH3:15])=[O:11]参加物
4
実験手順
A suspension of (S)-indoline-2-carboxylic acid (6.02 g., 36.9 mmol.) in ethanol (70 ml.) at 0° was saturated with hydrochloric acid and allowed to warm to room temperature. After 3 hours at room temperature, the resulting clear, red solution was purged with nitrogen and diluted with ethyl ether (200 ml.). The crystallized product was collected, washed with ethyl ether and dried in vacuo to give 6.43 g. of the title compound as white needles, m.p. 168°-169°; α!D =-70.7° (c=0.68, chloroform). TLC (ethyl acetate-hexane, 1:1) Rf =0.63 (as free base).
後処理
- customthe resulting clear, red solution was purged with nitrogen
- additiondiluted with ethyl ether (200 ml.)
- customThe crystallized product was collected
- washwashed with ethyl ether
- customdried in vacuo
- customto give 6.43 g
出典と根拠
- ORDレコード
- ord-2341f1275cda4573a992c40ec7d37def
- 出典データセット
- uspto-grants-1996_04
- 特許番号
- US05504080
反応ノート
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