HRID1095728

反应详情

EQUATION

反应方程式

HRID 1095728 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Palladium on carbon (10%, 0.876 g, 0.823 mmol) was added to a solution of (cis)-tert-butyl 4-azido-3-fluoropiperidine-1-carboxylate (2.01 g, 8.23 mmol) dissolved in THF and EtOH (1:1, 82 mL). The reaction was placed under a hydrogen atmosphere (balloon pressure) and stirred for 2 hours. The mixture was filtered through GF/F paper and concentrated in vacuo. The amine was purified on a Varian Bond Elut SCX column, eluting with methylene chloride followed by a solution of MeOH containing 6% aqueous NH4OH. The second eluant was concentrated in vacuo to provide the desired product (642 mg). MS ESI (+) m/z 218.8 (M+1) detected.

WORKUP

后处理

  1. filtrationThe mixture was filtered through GF/F paper
  2. concentrationconcentrated in vacuo
  3. customThe amine was purified on a Varian Bond Elut SCX column
  4. washeluting with methylene chloride
  5. concentrationThe second eluant was concentrated in vacuo