HRID1047771
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
PROCEDURE
实验过程
To a solution of 2-[2-(-1-ethyl-but-1-enyl)-3-methyl-benzoylamino]-indan-2-carboxylic acid ethyl ester (129) (270 mg, 0.72 mmol) in absolute EtOH (15 mL) is added the catalyst, Pd—C (50% wetted powder, 10% Pd, 46 mg, 2.2% mmol) under argon. The resulting reaction mixture is moved to the Paar apparatus to run hydrogenation: 50 psi, 70° C., overnight. The catalyst is removed by the filtration through a pre-column (10 g silica gel) and washed by EtOH. The combined EtOH solution is concentrated in vacuo. The residue is purified by HPLC to give a pure product (130) as white solid (75 mg, 28%).
WORKUP
后处理
- customThe resulting reaction mixture
- custom50 psi, 70° C., overnight
- customThe catalyst is removed by the filtration through a pre-column (10 g silica gel)
- washwashed by EtOH
- concentrationThe combined EtOH solution is concentrated in vacuo
- customThe residue is purified by HPLC