HRID1845999
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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
HOAc (2.47 mL, 42.7 mmol) was added dropwise to a mixture of 3,5-dichloropyridazin-4-amine (Preparation 4, 1000 mg, 6.098 mmol) and isopropylamine (7.27 mL, 85.4 mmol) cooled to 0° C. The resulting solid/suspension was heated under microwave irradiation at 105° C. for 5 hours. The reaction mixture was dissolved in minimum amount of MeOH and purified by silica gel column chromatography eluting with EtOAc:heptane: 10%-90% to provide the title compound as a slightly brownish solid in 74% yield, 2.52 g.
WORKUP
后处理
- temperatureThe resulting solid/suspension was heated under microwave irradiation at 105° C. for 5 hours
- custompurified by silica gel column chromatography
- washeluting with EtOAc