Mandelic Acid → HCID 13929038、化合物
反応式
[C:1]([OH:11])(=[O:10])[CH:2]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)[OH:3].[CH3:12][CH:13]1[CH2:18][CH2:17][CH2:16][NH:15][CH2:14]1>C(OCC)(=O)C>[C:1]([OH:11])(=[O:10])[CH:2]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)[OH:3].[CH3:12][C@H:13]1[CH2:18][CH2:17][CH2:16][NH:15][CH2:14]1参加物
4
実験手順
(+) mandelic acid (45.64 g, 0.3 mol) is dissolved in 300 ml of warm ethyl acetate. 3-methylpiperidine (29.8 g, 0.3 mol) is added under agitation and the solution allowed to return to ambient temperature. After 24 hours, the salt obtained is filtered and rinsed with an EA/AcOEt (1/1) mixture then recrystallized 3 times from AcOEt. In this way, the (S)-(+)-3-methylpiperidine mandelate salt (22.7 g) is obtained. M.p.=120-122° C; αD=+58.0° (methanol, c=1.0).
後処理
- customto return to ambient temperature
- customthe salt obtained
- filtrationis filtered
- washrinsed with an EA/AcOEt (1/1) mixture
- customthen recrystallized 3 times from AcOEt
出典と根拠
- ORDレコード
- ord-47395a219b794e2e8a6e8c534a55d801
- 出典データセット
- uspto-grants-2002_01
- 特許番号
- US06342511B1
反応ノート
読み込み中…