Water → Benzenamine, 5-methoxy-N-methyl-2-nitro-

HRID 33391

反応式

HRID 33391 の反応式
[CH3:1][NH2:2].F[C:4]1[CH:5]=[C:6]([O:13][CH3:14])[CH:7]=[CH:8][C:9]=1[N+:10]([O-:12])=[O:11].C(=O)([O-])[O-].[K+].[K+].O>C1COCC1.ClCCl>[CH3:14][O:13][C:6]1[CH:7]=[CH:8][C:9]([N+:10]([O-:12])=[O:11])=[C:4]([NH:2][CH3:1])[CH:5]=1

参加物

7

反応物 4

HCID 962WaterHCID 6329MethylamineHCID 11430Potassium CarbonateHCID 5656543-Fluoro-4-nitroanisole

生成物 1

HCID 153056Benzenamine, 5-methoxy-N-methyl-2-nitro-

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

83.5 mL (167.0 mmol) of a 2 molar solution of methylamine in THF are added dropwise to 14.3 g (83.56 mmol) 3-fluoro-4-nitro-anisol and 12.71 g (92.02 mmol) potassium carbonate in 200 mL dichloromethane. The mixture is stirred overnight and then combined with water. The organic phase is washed successively with water and ammonium chloride solution, dried and evaporated down. The yellow solid remaining is stirred with hexane. Yield: 12.7 g (84%); mass spectroscopy: [M+H]+=183.

後処理

  1. washThe organic phase is washed successively with water and ammonium chloride solution
  2. customdried
  3. customevaporated down
  4. stirringThe yellow solid remaining is stirred with hexane

出典と根拠

ORDレコード
ord-bc918e6a5f98444a864a487a48b4fb21
出典データセット
uspto-grants-2008_09
特許番号
US07429583B2

関連ノート

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