Methylamine → 3,4-Dimethoxy-N-methyl-5-nitrobenzamide

HRID 1401304ノート

反応式

HRID 1401304 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[C:10]([N+:14]([O-:16])=[O:15])[C:11]=1[O:12][CH3:13])[C:6](Cl)=[O:7].[CH3:17][NH2:18]>ClCCl>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[C:10]([N+:14]([O-:16])=[O:15])[C:11]=1[O:12][CH3:13])[C:6]([NH:18][CH3:17])=[O:7]

参加物

4

反応物 2

HCID 6329MethylamineHCID 219286153,4-Dimethoxy-5-nitrobenzoyl chloride

生成物 1

HCID 670370593,4-Dimethoxy-N-methyl-5-nitrobenzamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a stirred solution of 3,4-dimethoxy-5-nitro-benzoyl chloride (0.50 g, 2.04 mmol) in dichloromethane (10 mL) at 0° C., was added dropwise methylamine (1.02 mL, 2.04 mmol, 2 M in THF). The reaction mixture was stirred at room temperature till all starting material disappeared, then diluted with dichloromethane and washed with water. The organic phase was dried over anhydrous magnesium sulphate, filtered and evaporated to dryness to leave a crude residue that was recrystallised from a dichloromethane/isopropanol mixture to afford 3,4-dimethoxy-N-methyl-5-nitro-benzamide, 0.44 g (89%).

後処理

  1. washwashed with water
  2. dry with materialThe organic phase was dried over anhydrous magnesium sulphate
  3. filtrationfiltered
  4. customevaporated to dryness
  5. customto leave a crude residue that
  6. customwas recrystallised from a dichloromethane/isopropanol mixture

出典と根拠

ORDレコード
ord-2d617ad3986d4081b36b4d356662e667
出典データセット
uspto-grants-2014_12
特許番号
US08907099B2

反応ノート

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