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

HRID 1920080ノート

反応式

HRID 1920080 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-85c55b25cb5847c89b50f1e962adf583
出典データセット
uspto-grants-2012_05
特許番号
US08168793B2

反応ノート

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