Water → HCID 68089365、化合物

HRID 1772007ノート

反応式

HRID 1772007 の反応式
[N:1]1[C:10]2[C:5](=[CH:6][C:7]([NH:11][C:12](=[O:14])[CH3:13])=[CH:8][CH:9]=2)[N:4]=[CH:3][CH:2]=1.[H-].[Na+].I[CH3:18].O>C1COCC1>[CH3:18][N:11]([C:7]1[CH:6]=[C:5]2[C:10](=[CH:9][CH:8]=1)[N:1]=[CH:2][CH:3]=[N:4]2)[C:12](=[O:14])[CH3:13]

参加物

6

反応物 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 23273816HCID 23273816、化合物

生成物 1

HCID 68089365HCID 68089365、化合物収率 93%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of N-(quinoxalin-6-yl)acetamide (8.0 g, 0.043 mol) in THF (120 mL) was added sodium hydride (60% wt in mineral oil, 3.42 g, 0.086 mol). The mixture was stirred at room temperature for 10 min. Then iodomethane (7.28 g, 0.051 mol) was added. The mixture was stirred at room temperature for 2 h. Water (60 mL) was added carefully. The mixture was extracted with EtOAc (3×150 mL). The extracts were dried over sodium sulfate, concentrated to give N-methyl-N-(quinoxalin-6-yl)acetamide as a brown solid (8.04 g, yield 93%). ESI MS: m/z 202.1 [M+H]+.

後処理

  1. stirringThe mixture was stirred at room temperature for 2 h
  2. extractionThe mixture was extracted with EtOAc (3×150 mL)
  3. dry with materialThe extracts were dried over sodium sulfate
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-3177a101d5ef4114857646bc3a92a376
出典データセット
uspto-grants-2016_02
特許番号
US09249162B2

反応ノート

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