反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 50 °C
PROCEDURE
实验过程
0.18 g (0.26 mmol) (3R)-tert-butyl 3-(3,5-difluorophenyl)-5-oxo-4-(2-oxo-2-(2′-oxo-1′,2′,5,7-tetrahydrospiro[cyclopenta[b]pyridin-6,3′-pyrrolo[2,3-b]pyridin]-3-ylamino)ethyl)-8,11-dioxa-1,4-diazaspiro[5.6]dodecane-1-carboxylate were combined with 30 ml of a 1N methanolic hydrochloric acid solution and stirred for 1 h at 50° C. The reaction mixture was concentrated by rotary evaporation and purified by HPLC. The product fractions were evaporated down, neutralised with sodium hydrogen carbonate and the aqueous phase was extracted with DCM. The organic phase was concentrated by rotary evaporation. The residue was triturated with diethyl ether, suction filtered, washed with diethyl ether and dried.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated by rotary evaporation
- custompurified by HPLC
- customThe product fractions were evaporated down
- extractionthe aqueous phase was extracted with DCM
- concentrationThe organic phase was concentrated by rotary evaporation
- customThe residue was triturated with diethyl ether, suction
- filtrationfiltered
- washwashed with diethyl ether
- customdried