7-Fluoro-2-methylisatoicanhydride → Methyl 4-fluoro-2-(methylamino)benzoate

HRID 542797

反応式

HRID 542797 の反応式
[F:1][C:2]1[CH:14]=[CH:13][C:5]2[C:6](=[O:12])[O:7][C:8](=O)[N:9]([CH3:10])[C:4]=2[CH:3]=1.C[O-].[Na+]>CO>[F:1][C:2]1[CH:14]=[CH:13][C:5]([C:6]([O:7][CH3:8])=[O:12])=[C:4]([NH:9][CH3:10])[CH:3]=1

参加物

4

反応物 2

HCID 103302747-Fluoro-2-methylisatoicanhydrideHCID 10942334Sodium Methoxide

生成物 1

HCID 13474393Methyl 4-fluoro-2-(methylamino)benzoate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

A mixture of 7-fluoro-1-methyl-1H-3,1-benzoxazine-2,4-dione (20.0 g) and methanol (103 ml) was boiled under reflux. To the boiling mixture was added dropwise a solution of sodium methoxide (0.06 g) in methanol (50 ml.) during 19 minutes. The mixture was distilled in vacuo to remove solvent and give the product as a residue. There was thus obtained the novel compound methyl 4-fluoro-2-methylaminobenzoate as an oil which solidified on standing and was suitable for use in the next stage of synthesis. An analytical sample was prepared by distillation in vacuo followed by recrystallisation of the distillate from aqueous isopropanol. This sample had m.p. 39°-39.5°.

後処理

  1. temperatureunder reflux
  2. distillationThe mixture was distilled in vacuo
  3. customto remove solvent
  4. customgive the product as a residue

出典と根拠

ORDレコード
ord-f6a1bfbb73bb45619b016cb4f2ea1922
出典データセット
uspto-grants-1987_04
特許番号
US04659718

関連ノート

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