Water → N2-Methylpyridine-2,6-diamine

To a solution of 2,6-diaminopyridine (10 g, 91.63 mmol) in dry THF (100 mL) was added K2CO3 (18.8 g, 136.23 mmol) and CH3I (13 g, 91.63 mmol) and the reaction mixture was stirred at room temperature for 16 h. Water was added (10 mL) and the mixture was extracted with EtOAc (100 mL). The EtOAc layer was dried and was concentrated under reduced pressure. The residue was further purified by column chromatography (SiO2, 60-120, chloroform) to give 2-methylamino-6-aminopyridine (1.1 g, 10%) as a brown solid.

1. extractionthe mixture was extracted with EtOAc (100 mL)
2. dry with materialThe EtOAc layer was dried
3. concentrationwas concentrated under reduced pressure
4. customThe residue was further purified by column chromatography (SiO2, 60-120, chloroform)

ORD-Eintrag

ord-ade1abf3ede54fb393984d5aea9ced0f

Quelldatensatz

uspto-grants-2015_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09040541B2