HRID1621149
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
- 2.5 °C
PROCEDURE
实验过程
To a solution of benzoyl isocyanate (2 g, 12.2 mmol) in acetonitrile (40 mL) was added rapidly (diazomethyl)trimethylsilane (2M solution in hexane, 7.34 mL, 14.7 mmol) at 0-5° C., whereby the temperature rose to 15° C. (bubbling). The mixture was stirred at 0-5° C. for 1 h. Following solvent evaporation, the product was obtained after purification by flash chromatography (using silica gel and an ethyl acetate/heptane gradient) as yellow solid (1.84 g with 90% purity, 10.3 mmol, 84.0%) which was used without further purification for the next step.
WORKUP
后处理
- customrose to 15° C.
- custom(bubbling)
- customFollowing solvent evaporation
- customthe product was obtained
- customafter purification by flash chromatography (
- customan ethyl acetate/heptane gradient) as yellow solid (1.84 g with 90% purity, 10.3 mmol, 84.0%) which was used without further purification for the next step