HRID2121590
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
Heat a solution of 4-chloro-2,5,6-trimethyl-7-(2,4,6-trimethyl-phenyl)-7H-pyrrolo[2,3-d]pyrimidine (340 mg, 1.1 mmol) and N-(4-ethoxy-3-methoxy-phenethyl)-ethylenediamine in NMP (2 mL) for 14 h at 130° C. Pour into water (5 mL) and extract with EtOAc (2×10 mL). Dry the combined organic extracts over Na2SO4, filter, and concentrate under reduced pressure. Purify by preparative TLC, eluting with 10% MeOH in CH2Cl2. Dissolve the residue in a minimum amount of MeOH then add HCl in EtOAc (2 mL) and triturate with Et2O to obtain the title compound as a solid (HCl salt).
WORKUP
后处理
- extractionextract with EtOAc (2×10 mL)
- dry with materialDry the combined organic extracts over Na2SO4
- filtrationfilter
- concentrationconcentrate under reduced pressure
- customPurify by preparative TLC
- washeluting with 10% MeOH in CH2Cl2
- dissolutionDissolve the residue in a minimum amount of MeOH
- customadd HCl in EtOAc (2 mL) and triturate with Et2O