HRID1622965
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 70 °C
PROCEDURE
实验过程
To a solution of 1-aminocyclopentanecarboxylic acid (2.58 g, 19.97 mmol) in cyclopentanol (20 ml), was added concentrated sulfuric acid (2.15 g, 21.97 mmol) and the mixture stirred overnight at 70° C. The reaction was allowed to cool to RT and the cyclopentanol removed under reduced pressure. The residue was dissolved in EtOAc (30 ml) and washed with sat. NaHCO3 (30 ml) and water (3×20 ml) then dried (MgSO4), filtered and concentrated in vacuo to leave a dark yellow oil. Purification by column chromatography (15% 1.2 M NH3/MeOH in EtOAc) afforded the desired product (1.97 g, 50% yield).
WORKUP
后处理
- temperatureto cool to RT
- customthe cyclopentanol removed under reduced pressure
- dissolutionThe residue was dissolved in EtOAc (30 ml)
- washwashed with sat. NaHCO3 (30 ml) and water (3×20 ml)
- dry with materialthen dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated in vacuo
- customto leave a dark yellow oil
- customPurification by column chromatography (15% 1.2 M NH3/MeOH in EtOAc)