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レコード

ord-d912682f147b4f8cbce9c59b90853eca

出典データセット

uspto-grants-2014_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08748606B2