HRID1971839

反应详情

EQUATION

反应方程式

HRID 1971839 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionAfter completion of addition
  2. customThen the reaction was quenched
  3. additionby adding MeOH (2 ml)
  4. temperatureafter which it was warmed to room temperature
  5. dissolutionThe mixture was dissolved in EA
  6. washwashed with brine
  7. customdried
  8. customevaporated under reduced pressure
  9. customThe residue was purified by column chromatography (PE:EA=3:2)