HRID2121590

反应详情

EQUATION

反应方程式

HRID 2121590 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. extractionextract with EtOAc (2×10 mL)
  2. dry with materialDry the combined organic extracts over Na2SO4
  3. filtrationfilter
  4. concentrationconcentrate under reduced pressure
  5. customPurify by preparative TLC
  6. washeluting with 10% MeOH in CH2Cl2
  7. dissolutionDissolve the residue in a minimum amount of MeOH
  8. customadd HCl in EtOAc (2 mL) and triturate with Et2O