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

HRID 542797

Reaktionsgleichung

Reaktionsgleichung von HRID 542797
[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

Komponenten

4

Edukt 2

HCID 103302747-Fluoro-2-methylisatoicanhydrideHCID 10942334Sodium Methoxide

Produkt 1

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

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel2×

Versuchsvorschrift

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°.

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-f6a1bfbb73bb45619b016cb4f2ea1922
Quelldatensatz
uspto-grants-1987_04
Patentnummer
US04659718

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