HRID1378651

反应详情

EQUATION

反应方程式

HRID 1378651 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a well-stirred ice-bath-chilled solution of the racemic mixture of Step C (650 mg, 2.0 mmol) in anhydrous tetrahydrofuran (10 ml), a solution of lithium aluminum hydride in tetrahydrofuran (6.11 ml of a 1.0M solution, 6.11 mmol of lithium aluminum hydride) was added dropwise over 5 minutes. The reaction mixture was then stirred for 24 hours at ambient temperature before being ice-bath-chilled and cautiously quenched with 15% aqueous sodium hydroxide (2 ml). Anhydrous sodium sulfate was added to dry the mixture, which was then filtered. The filtrate was concentrated in vacuo to afford the title compound as a colorless oil in quantitative yield.

WORKUP

后处理

  1. temperaturebath-chilled
  2. customcautiously quenched with 15% aqueous sodium hydroxide (2 ml)
  3. additionAnhydrous sodium sulfate was added
  4. customto dry the mixture, which
  5. filtrationwas then filtered
  6. concentrationThe filtrate was concentrated in vacuo