6-Amino-3-chloropyridazine → 3-Amino-4-bromo-6-chloropyridazine

To a solution of 6-Chloro-pyridazin-3-ylamine (4 g, 31 mmol) in methanol (60 mL) was added NaHCO3 (5.2 g, 62 mmol). The reaction mixture was stirred for 30 minutes at RT then Br2 (4.9 g, 31 mmol) was added drop wise. Then the resulting reaction mixture was stirred additionally for 16 h at RT. After completion of reaction, the reaction mass concentrated under reduced pressure, crude purified by silica gel (100-200 mesh) chromatography using EtOAc/Hexane (8:2) to afford 4-Bromo-6-chloro-pyridazin-3-ylamine (2.3 g, 36%) as a solid.

1. customThen the resulting reaction mixture
2. stirringwas stirred additionally for 16 h at RT
3. customAfter completion of reaction
4. concentrationthe reaction mass concentrated under reduced pressure, crude
5. custompurified by silica gel (100-200 mesh) chromatography

ORDレコード

ord-4e3baff1832d4fa7abb52f3c6518eb96

出典データセット

uspto-grants-2014_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08822457B2