HRID11001
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
- -78 °C
PROCEDURE
实验过程
To Intermediate 18c (495.7 mg, 1.08 mmol) in THF at −78° C. was added LiHMDS (2.268 mL, 2.268 mmol) dropwise. After 10 min, tert-butyl bromoacetate was added and the mixture was stirred at −78° C. for 20 min. It was allowed to warm to −40° C. over 20 min, then quenched with NH4Cl. The reaction mixture was diluted with EtOAc, then washed with H2O, brine, dried (Na2SO4) and concentrated. It was purified by SiO2 chromatography (50% EtOAc/hexanes) to afford 367.9 mg (59%) of intermediate 38a.
WORKUP
后处理
- temperatureto warm to −40° C. over 20 min
- customquenched with NH4Cl
- additionThe reaction mixture was diluted with EtOAc
- washwashed with H2O, brine
- dry with materialdried (Na2SO4)
- concentrationconcentrated
- customIt was purified by SiO2 chromatography (50% EtOAc/hexanes)