Methylamine → 8-(N-Methyl)aminomethyl-10-methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazine

HRID 1059426Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1059426
Cl[CH2:2][C:3]1[CH:4]=[CH:5][C:6]2[S:11][C:10]3[N:12]=[CH:13][CH:14]=[N:15][C:9]=3[N:8]([CH2:16][O:17][CH3:18])[C:7]=2[CH:19]=1.[CH3:20][NH2:21]>CO>[CH3:20][NH:21][CH2:2][C:3]1[CH:4]=[CH:5][C:6]2[S:11][C:10]3[N:12]=[CH:13][CH:14]=[N:15][C:9]=3[N:8]([CH2:16][O:17][CH3:18])[C:7]=2[CH:19]=1

Komponenten

4

Edukt 2

HCID 6329MethylamineHCID 1133536310-methoxymethyl-8-chloromethyl-10H-pyrazino[2,3-b][1,4]benzothiazine

Produkt 1

HCID 186703078-(N-Methyl)aminomethyl-10-methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

8-Chloromethyl-10-methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazine was stirred in a solution of methylamine in methanol at room temperature over day and night. Then the reaction mixture was distilled under reduced pressure and the residue was distributed into sodium hydroxide and ethyl acetate. The organic layer was extracted and dried over anhydrous sodium sulfate. After distilling off the solvent under reduced pressure, the obtained residue was purified by silica gel column chromatography (eluted with dichloromethane/methanol) to thereby give the title compound as a yellow oily substance.

Aufarbeitung

  1. distillationThen the reaction mixture was distilled under reduced pressure
  2. extractionThe organic layer was extracted
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationAfter distilling off the solvent under reduced pressure
  5. customthe obtained residue was purified by silica gel column chromatography (eluted with dichloromethane/methanol)

Quellen und Nachweise

ORD-Eintrag
ord-1d5af62ee1cb45208655f8c0f8690b15
Quelldatensatz
uspto-grants-2003_02
Patentnummer
US06518423B1

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