HRID1445762
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
- 90 °C
PROCEDURE
实验过程
Add acetic anhydride (0.97 mmol) and pyridine (0.58 mmol) to a round bottom flask containing 4-benzyloxy-2-(4-bromo-2-fluoro-benzoylamino)-butyric acid (1.0 mmol) (See Intermediate 35) and heat to 90° C. for two hours. After this time, remove the heat and concentrate in vacuo. Wash crude with 1N hydrochloric acid and water while extracting with diethyl ether. Concentrate the organics in vacuo and purify on an Isco CombiFlash® chromatography system eluting with ethyl acetate and hexane. MS (m/e) (79Br/81Br): 408.3/410.3 (M+1)
WORKUP
后处理
- customAfter this time, remove the
- temperatureheat
- concentrationconcentrate in vacuo
- washWash crude with 1N hydrochloric acid and water
- extractionwhile extracting with diethyl ether
- concentrationConcentrate the organics in vacuo
- custompurify on an Isco CombiFlash® chromatography system
- washeluting with ethyl acetate and hexane