HRID1426537

反应详情

EQUATION

反应方程式

HRID 1426537 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3-[5-(7-[2-(trimethylsilyl)ethoxy]methyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1,3-thiazol-2-yl]pentanedinitrile (14 mg, 0.033 mmol) in DCM (3 mL) containing TFA (0.6 mL) was stirred for 4 hours. The mixture was then concentrated and the residue was redissolved in methanol (2 mL) to which ethylenediamine (0.4 mL) was then added. After 1 hour reaction time, the product was purified by preparative-HPLC/MS (C18 eluting with a gradient of ACN/H2O containing 0.15% NH4OH) to afford the desired product (6 mg, 62%).

WORKUP

后处理

  1. concentrationThe mixture was then concentrated
  2. dissolutionthe residue was redissolved in methanol (2 mL) to which ethylenediamine (0.4 mL)
  3. additionwas then added
  4. customAfter 1 hour reaction time
  5. customthe product was purified by preparative-HPLC/MS (C18
  6. washeluting with a gradient of ACN/H2O containing 0.15% NH4OH)