Methylamine → 2-Amino-5-fluoro-N-methylbenzamide

HRID 62485

Reaktionsgleichung

Reaktionsgleichung von HRID 62485
[F:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:10]C(=O)[O:8][C:7](=O)[C:6]=2[CH:13]=1.[CH3:14][NH2:15]>O1CCCC1>[NH2:10][C:5]1[CH:4]=[CH:3][C:2]([F:1])=[CH:13][C:6]=1[C:7]([NH:15][CH3:14])=[O:8]

Komponenten

4

Edukt 2

HCID 6329MethylamineHCID 2885605-Fluoroisatoic anhydride

Produkt 1

HCID 431325582-Amino-5-fluoro-N-methylbenzamideAusbeute 65 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

6-Fluoro-2H-3,1-benzoxazine-2,4(1H)-dione (200 mg, 1.104 mmol) was dissolved in dry tetrahydrofuran (THF) (10 mL), at which time methyl amine (3.31 mL, 6.63 mmol) was added. The reaction was stirred at room temperature for 1 h, then concentrated under vacuum. The crude product was purified on silica (Biotage, 40% EtOAc/hexene) to afford the title compound (120 mg, 65%) as a white solid. LC-MS (ES) m/z=169.1 (M+H)+

Aufarbeitung

  1. additionwas added
  2. concentrationconcentrated under vacuum
  3. customThe crude product was purified on silica (Biotage, 40% EtOAc/hexene)

Quellen und Nachweise

ORD-Eintrag
ord-aef9e4fc5a7a44e5a961eff5a775f7f9
Quelldatensatz
uspto-grants-2016_09
Patentnummer
US09446034B2

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