HRID844240

反应详情

EQUATION

反应方程式

HRID 844240 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

To a solution of compound (ii), above, (380 mg, 1.4 mmol) in THF (5 mL) at −78° C. was added n-BuLi (1 mL, 1.6 M sol. in hexane, 1.6 mmol). The mixture was stirred at −78° C. for 20 min. Tetrahydro-4H-pyran-4-one (280 mg, 2.8 mmol) dissolved in THF (1 mL) was added and the reaction mixture stirred at −78° C. for 2 hrs. The mixture was then quenched with NH4Cl (saturated) and extracted with ethyl acetate. The organic extract was washed with brine and dried over anhydrous Na2SO4. The crude residue was purified by flash chromatography to give the title product as a yellow solid (150 mg, 37% yield).

WORKUP

后处理

  1. additionwas added
  2. stirringthe reaction mixture stirred at −78° C. for 2 hrs
  3. customThe mixture was then quenched with NH4Cl (saturated)
  4. extractionextracted with ethyl acetate
  5. extractionThe organic extract
  6. washwas washed with brine
  7. dry with materialdried over anhydrous Na2SO4
  8. customThe crude residue was purified by flash chromatography