HRID1947270
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
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
To a solution of methyl 4-[4-(cyclohexylamino)-8-(4-iodobenzyl)-2-oxo-1,3,8-triazaspiro[4.5]dec-3-en-1-yl]butanoate (Intermediate I.3.a.1, 150 mg, 0.29 mmol), zinc cyanide (24 mg, 0.20 mmol) in DMF (3 mL) was added tetrakis (33 mg, 0.03 mmol). The resulting solution was allowed to stir at 80° C. for 16 h. After 16 h, the reaction mixture was filtered, concentrated in vacuo and purified by reverse phase preparative HPLC (5- 95% MeCN/H2O containing 0.1% TFA, C18) to provide the desired product. LRMS (M+1)=466.6.
WORKUP
后处理
- waitAfter 16 h
- filtrationthe reaction mixture was filtered
- concentrationconcentrated in vacuo
- custompurified by reverse phase preparative HPLC (5- 95% MeCN/H2O containing 0.1% TFA, C18)