HRID1421039
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 4-bromo-3,6-dichloro-pyridazine (1.11 g, 5 mmol), (J.Chem. Soc., Perkin Trans I, 1974, 696), and 2-(methylamino)ethanol (0.75 g, 10 mmol) in isopropanol (10 ml) was heated at reflux for 30 minutes. The solvent was removed by evaporation, the residue was partitioned between methylene chloride and water and the aqueous layer was adjusted to pH9 with solid potassium carbonate. The organic layer was separated, washed with brine, dried (MgSO4) and the solvent removed by evaporation. The residue was triturated with ether, collected by filtration and dried under vacuum to give 2-(N-(3,6-dichloropyridazin-4-yl)-N-methylamino)ethanol (1 g, 90%).
WORKUP
后处理
- temperatureat reflux for 30 minutes
- customThe solvent was removed by evaporation
- customthe residue was partitioned between methylene chloride and water
- customThe organic layer was separated
- washwashed with brine
- dry with materialdried (MgSO4)
- customthe solvent removed by evaporation
- customThe residue was triturated with ether
- filtrationcollected by filtration
- customdried under vacuum