HRID1473459
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
- 90 °C
PROCEDURE
实验过程
A microwave vial was charged with 1-(2-bromo-4-(trifluoromethyl)phenyl)-N-(2,4-dimethoxybenzyl)-N-(thiazol-2-yl)isoquinoline-6-sulfonamide (see Example 70, step 3; 0.185 g, 0.278 mmol), Pd(PPh3)4 (0.016 g, 0.014 mmol), and DMF (0.557 ml). Allyltributyltin (0.104 ml, 0.334 mmol) was added and the reaction was heated in a microwave reactor at 90° C. for 30 minutes. The reaction was concentrated and purified via column chromatography (40 g silica gel column, gradient elution 0 to 50% EtOAc:Heptane) to afford 1-(2-allyl-4-(trifluoromethyl)phenyl)-N-(2,4-dimethoxybenzyl)-N-(thiazol-2-yl)isoquinoline-6-sulfonamide as a light pink solid. m/z (ESI) 626.3 (M+H)+.
WORKUP
后处理
- concentrationThe reaction was concentrated
- custompurified via column chromatography (40 g silica gel column, gradient elution 0 to 50% EtOAc:Heptane)