HRID42759

反应详情

EQUATION

反应方程式

HRID 42759 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), to a ice-cold solution of 3-(2-methyl-[1,3]dioxolan-2-yl)-benzaldehyde (896 mg, 4.66 mmol) in MeOH (10.0 mL) was added NaBH4 (228 mg, 5.79 mmol in four equal portion). The reaction mixture was then stirred for 1 h at rt. Water was added and the mixture was extracted twice with EA. The combined org. extracts were washed with brine, dried over Na2SO4, filtered, and the solvent was removed under reduced pressure to give the title compound as a colorless oil: TLC:rf (50:50 hept-EA)=0.28. LC-MS-conditions 02: tR=0.74 min; [M+H]+=195.71.

WORKUP

后处理

  1. extractionthe mixture was extracted twice with EA
  2. washextracts were washed with brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. customthe solvent was removed under reduced pressure