HRID1817560
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
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
- concentrationThe mixture was then concentrated
- dissolutionthe residue was redissolved in methanol (2 mL) to which ethylenediamine (0.4 mL)
- additionwas then added
- customAfter 1 hour reaction time
- customthe product was purified by preparative-HPLC/MS (C18
- washeluting with a gradient of ACN/H2O containing 0.15% NH4OH)