HRID571372
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
- 65 °C
PROCEDURE
实验过程
A suspension of NaOAc (1.415 g, 17.25 mmol), Pd(dppf)C12 (0.841 g, 1.150 mmol) and 6-chloro-3-iodo-1-trityl-1H-pyrazolo[4,3-c]pyridine (6 g, 11.50 mmol) in MeOH (30 ml) was stirred under CO (120 psi) at 65° C. for 3 days. After reaction, the reaction mixture was diluted with DCM and dry loaded on silica column and purified by column chromatography on silica gel 120 g, eluting with 1:3 EA in Hexane to give the desired product as an off white solid 4.74 g (91% yield). MS ESI calc'd. for C27H20ClN3O2 [M+1]+ 454, found 454.
WORKUP
后处理
- customAfter reaction
- customdry
- custompurified by column chromatography on silica gel 120 g
- washeluting with 1:3 EA in Hexane