HRID1970450
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
A solution of 1.71 g 4-[(S)-3-tert-butoxycarbonylamino-2-(9H-fluoren-9-ylmethoxycarbonylamino)-propionyl]-piperazine-1-carboxylic acid ethyl ester in 50 ml THF was stirred in the presence of 4 ml 1-octanethiol and 90 μl DBU. After 12 h the mixture was concentrated, the residue dissolved in dichloromethane and extracted with 0.1 M HCl. The aqueous phase was brought to pH9 by adding aqueous NaHCO3 before being extracted with dichloromethane. The product was obtained after evaporation of the solvent and was used in the subsequent reaction.
WORKUP
后处理
- concentrationAfter 12 h the mixture was concentrated
- dissolutionthe residue dissolved in dichloromethane
- extractionextracted with 0.1 M HCl
- additionby adding aqueous NaHCO3
- extractionbefore being extracted with dichloromethane
- customThe product was obtained
- customafter evaporation of the solvent
- customwas used in the subsequent reaction