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
- 0 °C
PROCEDURE
实验过程
Sodium bis(trimethylsilyl)amide (2 mL, 4 mmol, 2M in THF) was added to a stirred suspension of (methoxymethyl)triphenylphosphonium chloride (1.47 g, 4.3 mmol) in dry THF (20 mL) at 0° C. for 35 min and a solution of 5-Oxo-5,6,7,8-tetrahydronaphthalene-1-carbonitrile [prepared from 5-bromo-tetralone following the procedure described in PCT publication WO2004/071389A2, Intermediate 41](490 mg, 2.86 mmol) in THF (10 mL) added over 10 min. The mixture was stirred at 0° C. for 2 h and at room temperature for 1 h. Water was added and the mixture was partitioned between EtOAc and brine. The organic layer was dried and concentrated. The crude product was purified via preparative-TLC (PE:EtOAc=10:1) to afford the title compound.
WORKUP
后处理
- additionadded over 10 min
- customthe mixture was partitioned between EtOAc and brine
- customThe organic layer was dried
- concentrationconcentrated
- customThe crude product was purified via preparative-TLC (PE:EtOAc=10:1)