HRID40281
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
- 35 °C
PROCEDURE
实验过程
To a stirring solution of (R,Z)—N-(4-bromo-2-chlorobenzylidene)-2-methylpropane-2-sulfinamide (1370 mg, 4246 μmol) and (trifluoromethyl)trimethylsilane (943 μl, 6369 μmol) in DMF (5 mL) was added 1,3-bis(1-adamantyl)imidazol-2-ylidene (143 mg, 425 μmol). Reaction stirred at 35° C. for 18 h then quenched with sat NH4Cl (10 mL). Reaction partitioned between EtOAc (40 mL) and 5% NaHCO3 (10 mL). Organic dried over MgSO4, concentrated to and oil from toluene, then purified on silica (80 g) eluting with 20>30% EtOAc/Hex. Product isolated as a white solid.
WORKUP
后处理
- customReaction
- customthen quenched with sat NH4Cl (10 mL)
- customReaction
- custompartitioned between EtOAc (40 mL) and 5% NaHCO3 (10 mL)
- dry with materialOrganic dried over MgSO4
- concentrationconcentrated to and oil from toluene
- custompurified on silica (80 g)
- washeluting with 20>30% EtOAc/Hex
- customProduct isolated as a white solid