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
- 150 °C
PROCEDURE
实验过程
Trifluoromethane sulfonic acid 1-ethyl-3,3,5-trimethyl-2,4-dioxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepine-7-yl ester(0.59 g), 2-(but-3-ynyl)isoindol-1,3-dione(0.3 g), dichlorobis(triphenyl phosphine)palladium (II) (53 mg), copper(I) iodide(29 mg), and triethylamine(0.39 ml) were added to DMF(4 ml). The mixture was heated at 150° C. (microwave reactor) for 10 minutes. The reaction liquid was cooled to room temperature, and subjected to celite filtration. The filtrate was condensed under reduced pressure and the residue was purified by silica gel column chromatography (hexane: ethyl acetate=60:40→30:70). The purified product was condensed under reduced pressure to give the title compound(0.51 g) as a yellowish-white solid.
WORKUP
后处理
- customThe reaction liquid
- temperaturewas cooled to room temperature
- filtrationsubjected to celite filtration
- customcondensed under reduced pressure
- customthe residue was purified by silica gel column chromatography (hexane: ethyl acetate=60:40→30:70)
- customcondensed under reduced pressure