HRID2354815
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
Lithium hydroxide monohydrate (0.066 g, 1.57 mmol) was added to a solution of 2-{4-[6-(2-cyclopropylethylcarbamoyl)pyridazin-3-yl]piperazine-1-carbonyl}benzoic acid methyl ester (0.230 g) in tetrahydrofuran (10 mL) and water (5 mL) stirred at ambient temperature overnight. THF was removed in vacuo, the residue was dissolved in ethyl acetate (100 mL), neutralized by addition of 5% HCl solution, washed with brine, dried over anhydrous Na2SO4 and concentrated. The residue was recrystallized from dichloromethane and hexanes to yield 0.107 g of the title compound (42% yield).
WORKUP
后处理
- customTHF was removed in vacuo
- dissolutionthe residue was dissolved in ethyl acetate (100 mL)
- additionneutralized by addition of 5% HCl solution
- washwashed with brine
- dry with materialdried over anhydrous Na2SO4
- concentrationconcentrated
- customThe residue was recrystallized from dichloromethane and hexanes