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

HRID 1841508노트

반응식

HRID 1841508 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-121255f691e34b9baa67cd7e793cfa3f
출처 데이터셋
uspto-grants-2004_01
특허 번호
US06683184B2

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