HRID1878311

反应详情

EQUATION

反应方程式

HRID 1878311 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customHCl gas is bubbled through the reaction mixture for 20 min
  2. customsolvent is removed under reduced pressure
  3. dissolutionThe residue is redissolved in 3:1 chloroform/isopropanol (100 mL)
  4. customThe layers are separated
  5. extractionthe aqueous layer is extracted with ethyl acetate (3×50 mL)
  6. concentrationThe combined organic layers are concentrated
  7. customtriturated with methanol