HRID1878311
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
5-Bromo-N-(5-(2-methoxy-6-(4-methoxybenzyloxy)phenyl)-1H-pyrazol-3-yl)pyrazin-2-amine (3.1 g, 6.43 mmol) is dissolved in MeOH (100 mL). HCl gas is bubbled through the reaction mixture for 20 min. The mixture is stirred for 2 h and solvent is removed under reduced pressure. The residue is redissolved in 3:1 chloroform/isopropanol (100 mL) and combined with saturated NaHCO3 solution (100 mL). The layers are separated and the aqueous layer is extracted with ethyl acetate (3×50 mL). The combined organic layers are concentrated and triturated with methanol to give 1.5 g (64%) of a brown solid.
WORKUP
后处理
- customHCl gas is bubbled through the reaction mixture for 20 min
- customsolvent is removed under reduced pressure
- dissolutionThe residue is redissolved in 3:1 chloroform/isopropanol (100 mL)
- customThe layers are separated
- extractionthe aqueous layer is extracted with ethyl acetate (3×50 mL)
- concentrationThe combined organic layers are concentrated
- customtriturated with methanol