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

HRID 2236623ノート

反応式

HRID 2236623 の反応式
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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-ffcd082288644aaeb3eaacea2ecc158f
出典データセット
uspto-grants-2010_05
特許番号
US07713994B2

反応ノート

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