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
- 100 °C
PROCEDURE
实验过程
A mixture of bromobenzene (300 mg), (S)-2-methylpiperazine (230 mg), (S)-(−)-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (BINAP) (48 mg), sodium tert-butoxide (266 mg), tris-(dibenzylideneacetone)dipalladium(0) (26 mg) and toluene (15 ml) was stirred at 100° C. for 4 hours under a nitrogen atmosphere. The mixture was cooled to room temperature and saturated aqueous sodium hydrogencarbonate solution was added thereto. The organic layer was separated, washed with brine and dried over magnesium sulfate. The solvent was removed under reduced pressure. The obtained crude product was purified by silica gel column chromatography (chloroform-methanol 20:1) to give the title compound in a pure form.
WORKUP
后处理
- temperatureThe mixture was cooled to room temperature
- customThe organic layer was separated
- washwashed with brine
- dry with materialdried over magnesium sulfate
- customThe solvent was removed under reduced pressure
- customThe obtained crude product
- customwas purified by silica gel column chromatography (chloroform-methanol 20:1)