Mandelic Acid → HCID 13929038, 화합물
반응식
[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]1참가 물질
4
실험 절차
(+) 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).
후처리
- customto return to ambient temperature
- customthe salt obtained
- filtrationis filtered
- washrinsed with an EA/AcOEt (1/1) mixture
- customthen recrystallized 3 times from AcOEt
출처 및 근거
- ORD 기록
- ord-47395a219b794e2e8a6e8c534a55d801
- 출처 데이터셋
- uspto-grants-2002_01
- 특허 번호
- US06342511B1
반응 노트
불러오는 중…