Methyl iodide → 1-[(2-Methoxynaphth-3-yl)-N-methylaminocarbonyl]-4-(3,5-dimethylphenyl)piperazine

HRID 1841508ノート

反応式

HRID 1841508 の反応式
[CH3:1][O:2][C:3]1[C:12]([NH:13][C:14]([N:16]2[CH2:21][CH2:20][N:19]([C:22]3[CH:27]=[C:26]([CH3:28])[CH:25]=[C:24]([CH3:29])[CH:23]=3)[CH2:18][CH2:17]2)=[O:15])=[CH:11][C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=1.[H-].[Na+].[CH3:32]I>CN(C)C=O>[CH3:1][O:2][C:3]1[C:12]([N:13]([CH3:32])[C:14]([N:16]2[CH2:21][CH2:20][N:19]([C:22]3[CH:23]=[C:24]([CH3:29])[CH:25]=[C:26]([CH3:28])[CH:27]=3)[CH2:18][CH2:17]2)=[O:15])=[CH:11][C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=1

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 234462211-[(2-Methoxynaphth-3-yl)aminocarbonyl]-4-(3,5-dimethylphenyl)piperazine

生成物 1

HCID 234463591-[(2-Methoxynaphth-3-yl)-N-methylaminocarbonyl]-4-(3,5-dimethylphenyl)piperazine収率 86.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To 1-[(2-methoxynaphth-3-yl)aminocarbonyl]-4-(3,5-dimethylphenyl)piperazine (210 mg, 0.54 mmol) dissolved in dimethylformamide (15 ml), 60% sodium hydride (21.5 mg, 0.54 mmol) was added, stirred at room temperature for 15 minutes, and thereto methyl iodide (76.6 mg, 0.54 mmol) was added. The resulting mixture was stirred at room temperature for 6 hours, concentrated under the reduced pressure to remove the solvent and purified by column chromatography to obtain the titled compound.

後処理

  1. stirringThe resulting mixture was stirred at room temperature for 6 hours
  2. concentrationconcentrated under the reduced pressure
  3. customto remove the solvent
  4. custompurified by column chromatography

出典と根拠

ORDレコード
ord-121255f691e34b9baa67cd7e793cfa3f
出典データセット
uspto-grants-2004_01
特許番号
US06683184B2

反応ノート

読み込み中…