HRID2112549

反应详情

EQUATION

反应方程式

HRID 2112549 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The 4-[(1,3-dioxoisoindolin-2-yl)methyl]-4-fluoropiperidinecarboxylic acid tert-butyl ester was dissolved in ethanol (200 mL), and then hydrazine monohydrate (10.0 mL) was added. After stirring at room temperature for 2 hours, the precipitated solid was filtered out and the filtrate was concentrated under reduced pressure. The obtained crudely purified product was further purified by silica gel column chromatography (5% MeOH/CH2Cl2) to obtain 4-(aminomethyl)-4-fluoropiperidinecarboxylic acid tert-butyl ester. The compound was identified by 1H-NMR. The yield was 3.23 g (76%).

WORKUP

后处理

  1. filtrationthe precipitated solid was filtered out
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe obtained crudely purified product
  4. customwas further purified by silica gel column chromatography (5% MeOH/CH2Cl2)