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
- 120 °C
PROCEDURE
实验过程
To a solution of (S)-ethyl 2-tert-butoxy-2-(7-(4-chlorophenyl)-2-(2-chloropyridin-4-yl)-5-methylbenzo[d]thiazol-6-yl)acetate (48 mg, 0.091 mmol) in microwave vial, was added 1-methyl-5-(tributylstannyl)-1H-pyrazolo[4,3-b]pyridine (47 mg, 0.111 mmol), copper(I) iodide (9 mg, 0.045 mmol), lithium chloride (11 mg, 0.27 mmol), Pd(PPh3)4 (10 mg, 0.009 mmol). The reaction mixture was heated at 120° C. for 4 hours. Then the mixture was washed by saturated NaHCO3, extracted by EtOAc, the organic phase was dried over MgSO4, filtered, concentrated down, purified by silica gel column, eluting by 0-60% EtOAc in hexanes to give the product. LCMS-ESI+: calc'd for C34H32ClN5O3S: 626.2 (M+H+); found: 626.3.
WORKUP
后处理
- washThen the mixture was washed by saturated NaHCO3
- extractionextracted by EtOAc
- dry with materialthe organic phase was dried over MgSO4
- filtrationfiltered
- concentrationconcentrated down
- custompurified by silica gel column
- washeluting by 0-60% EtOAc in hexanes
- customto give the product