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 1-{[(S)-2-(3-Trifluoromethoxy-phenylcarbamoyl)-pyrrolidine-1-carbonyl]-amino}-indolizine-3-carboxylic acid benzyl ester (100 mg, 0.177 mmol) dissolved in THF (3 mL) was added Pd/C 10% (20 mg). Air was removed from the flask under vacuum and replaced with nitrogen three times, finally nitrogen was removed and replaced with hydrogen and the mixture was stirred at RT for 5 h. Hydrogen was removed and replaced by nitrogen, the catalyst was removed by filtration through a pad of Celite and washed with THF. Solvents were concentrated to give a mixture containing the desired compound contaminated with 20% of the decarboxylated analog. The mixture was used without further purification in the next step. LC/MS: 475 [M−H]−; tR (HPLC conditions a): 3.41 min.
WORKUP
后处理
- customAir was removed from the flask under vacuum
- customwas removed
- customHydrogen was removed
- customthe catalyst was removed by filtration through a pad of Celite
- washwashed with THF
- concentrationSolvents were concentrated
- customto give a mixture