Methylamine → Benzoic acid, 2-(methylamino)-3-nitro-, methyl ester

HRID 1773741

反応式

HRID 1773741 の反応式
F[C:2]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].C(=O)([O-])[O-].[K+].[K+].[CH3:21][NH2:22]>C(Cl)Cl.O>[CH3:21][NH:22][C:2]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5]

参加物

6

反応物 3

HCID 6329MethylamineHCID 11430Potassium CarbonateHCID 13470961Methyl 2-fluoro-3-nitrobenzoate

生成物 1

HCID 59635415Benzoic acid, 2-(methylamino)-3-nitro-, methyl ester

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

Methyl 2-fluoro-3-nitrobenzoate (25 g, 0.126 mol) was dissolved in DCM (400 ml) and to this was added Potassium carbonate (34.7 g, 0.25 mol) followed by Methylamine (20.63 ml, 0.5 mol). Reaction was stirred at room temperature under argon. Upon completion reaction was diluted with water and extracted with DCM (3×) then dried over magnesium sulfate. Solvents were removed under reduced pressure to afford methyl 2-(methylamino)-3-nitrobenzoate as a yellow solid.

後処理

  1. customReaction
  2. customUpon completion reaction
  3. extractionextracted with DCM (3×)
  4. dry with materialthen dried over magnesium sulfate
  5. customSolvents were removed under reduced pressure

出典と根拠

ORDレコード
ord-7b54cf94915f4dfb8c875f28ccffe5d3
出典データセット
uspto-grants-2016_02
特許番号
US09255089B2

関連ノート

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