HRID1971839
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
- -70 °C
PROCEDURE
实验过程
The solution of the product of example 87 (830 mg, 2.5 mmol) in toluene (5 ml) was cooled down to −70° C. DIBAL-H (1 mol/l in toluene, 3.12 ml) was added dropwise. After completion of addition, the mixture was stirred at −70° C. for one hour. Then the reaction was quenched by adding MeOH (2 ml), after which it was warmed to room temperature. The mixture was dissolved in EA, washed with brine, dried and evaporated under reduced pressure. The residue was purified by column chromatography (PE:EA=3:2) to afford the title compound (355 mg, 47% yield).
WORKUP
后处理
- additionAfter completion of addition
- customThen the reaction was quenched
- additionby adding MeOH (2 ml)
- temperatureafter which it was warmed to room temperature
- dissolutionThe mixture was dissolved in EA
- washwashed with brine
- customdried
- customevaporated under reduced pressure
- customThe residue was purified by column chromatography (PE:EA=3:2)