Sodium Acetate → (3Z)-3-{1-[(3-hydroxy-4-methoxybenzyl)amino]ethylidene}-4-phenylpiperidine-2,6-dione

HRID 2236623노트

반응식

HRID 2236623 반응식
O/[C:2](=[C:4]1\[C:5](=[O:17])[NH:6][C:7](=[O:16])[CH2:8][CH:9]\1[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)/[CH3:3].[NH2:18][CH2:19][C:20]1[CH:21]=[CH:22][C:23]([O:27][CH3:28])=[C:24]([OH:26])[CH:25]=1.C([O-])(=O)C.[Na+]>C(O)C>[OH:26][C:24]1[CH:25]=[C:20]([CH:21]=[CH:22][C:23]=1[O:27][CH3:28])[CH2:19][NH:18]/[C:2](=[C:4]1\[C:5](=[O:17])[NH:6][C:7](=[O:16])[CH2:8][CH:9]\1[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)/[CH3:3]

참가 물질

5

반응물 3

HCID 517045Sodium AcetateHCID 11329985-(Aminomethyl)-2-methoxyphenolHCID 68694730(3Z)-3-(1-hydroxyethylidene)-4-phenylpiperidine-2,6-dione

생성물 1

HCID 59300292(3Z)-3-{1-[(3-hydroxy-4-methoxybenzyl)amino]ethylidene}-4-phenylpiperidine-2,6-dione수율 89.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a suspension of (3Z)-3-(1-hydroxyethylidene)-4-phenylpiperidine-2,6-dione (0.12 g, 0.52 mmol) and 5-(aminomethyl)-2-methoxyphenol (98 mg, 0.52 mmol) in absolute ethanol (5 mL) is added sodium acetate (0.75 mmol). The mixture is heated at reflux overnight and then allowed to cool to room temperature. The solvent is evaporated under reduced pressure and the residue is triturated with diethyl ether. The solid is collected, washed with diethyl ether, water, and methanol, and dried under vacuum to give (3Z)-3-{1-[(3-hydroxy-4-methoxybenzyl)amino]ethylidene}-4-phenylpiperidine-2,6-dione as a white powder (0.17 g, 88%).

후처리

  1. temperatureThe mixture is heated
  2. temperatureat reflux overnight
  3. customThe solvent is evaporated under reduced pressure
  4. customthe residue is triturated with diethyl ether
  5. customThe solid is collected
  6. washwashed with diethyl ether, water, and methanol
  7. customdried under vacuum

출처 및 근거

ORD 기록
ord-ffcd082288644aaeb3eaacea2ecc158f
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07713994B2

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