HRID1986377
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
- 175 °C
PROCEDURE
实验过程
Under Ar, a suspension of the product from Example 9, Step 2 (50 mg, 162 μmol) in DME (1.4 mL) and toluene (2.8 mL) was treated with tris(dibenzylidene-acetone)dipalladium (15 mg, 16 μmol), racemic-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (20 mg, 32 μmol), N-(3-mercaptophenyl)acetamide (32.6 mg, 195 μmol), and sodium tert-butoxide (22 mg, 227 μmol). This mixture was then heated to 175° C. by microwave for 15 min. After cooling to rt, the reaction mixture was diluted with ethyl acetate (30 ml), filtered through a celite pad and the filtrate was concentrated in vacuo. The residue was purified by reverse phase HPLC to give the title compound (17 mg, 26%). MS (ES+) m/e 396 [M+H]+.
WORKUP
后处理
- temperatureAfter cooling to rt
- filtrationfiltered through a celite pad
- concentrationthe filtrate was concentrated in vacuo
- customThe residue was purified by reverse phase HPLC