HRID1622965

反应详情

EQUATION

反应方程式

HRID 1622965 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureto cool to RT
  2. customthe cyclopentanol removed under reduced pressure
  3. dissolutionThe residue was dissolved in EtOAc (30 ml)
  4. washwashed with sat. NaHCO3 (30 ml) and water (3×20 ml)
  5. dry with materialthen dried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customto leave a dark yellow oil
  9. customPurification by column chromatography (15% 1.2 M NH3/MeOH in EtOAc)