HRID29755

反应详情

EQUATION

反应方程式

HRID 29755 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Periodinane (26.9 g, 63.5 mmol) was added to 4-Hydroxymethyl-piperidine-1-carboxylic acid tert-butyl ester (10.5 g, 48.8 mmol) in CH2Cl2 (200 mL) and stirred for 90 min. Diethyl ether (560 mL) was added and precipitates were removed by extraction with 10% Na2S2O3/saturated NaHCO3 (1:1, 300 mL). The organic layer was washed with 0.5 M NaOH solution and brine. The organic phase was dried and concentrated under reduced pressure. Purification using flash chromatography (hexane/EtOAc, 8:2) gave 4-Formyl-piperidine-1-carboxylic acid tert-butyl ester (8.5 g, 81%).

WORKUP

后处理

  1. customprecipitates
  2. customwere removed by extraction with 10% Na2S2O3/saturated NaHCO3 (1:1, 300 mL)
  3. washThe organic layer was washed with 0.5 M NaOH solution and brine
  4. customThe organic phase was dried
  5. concentrationconcentrated under reduced pressure
  6. customPurification