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

HRID 542797

반응식

HRID 542797 반응식
[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

참가 물질

4

반응물 2

HCID 103302747-Fluoro-2-methylisatoicanhydrideHCID 10942334Sodium Methoxide

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

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°.

후처리

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

출처 및 근거

ORD 기록
ord-f6a1bfbb73bb45619b016cb4f2ea1922
출처 데이터셋
uspto-grants-1987_04
특허 번호
US04659718

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