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 record

ord-bdd68b501c7a44a1b4f3e0f0ea013f9f

Source dataset

uspto-grants-2011_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07982036B2