HRID545338
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
CONDITIONS
反应条件
- 温度
- 110 °C
PROCEDURE
实验过程
To 0.15 g (0.4 mmol) of 2-[cyclopropyl-(4-trifluoromethoxy-benzoyl)-amino]-3-oxo-butyric acid ethyl ester in 5 ml of MeOH was added 0.2 g (1.5 mmol) of ammonium trifluoroacetate. The MeOH was evaporated and the residue heated to 110° C. for 4 h. The cooled residue was partitioned between saturated sodium hydrogen carbonate solution and CH2Cl2. The organic phase was dried with sodium sulfate and concentrated. Purification by flash column chromatography [n-heptane/EtOAc 3:7 to 1:1] afforded 0.1 g (73%) of the title compound as a colorless solid. MS: 355.2 (MH+).
WORKUP
后处理
- customThe MeOH was evaporated
- customThe cooled residue was partitioned between saturated sodium hydrogen carbonate solution and CH2Cl2
- dry with materialThe organic phase was dried with sodium sulfate
- concentrationconcentrated
- customPurification by flash column chromatography [n-heptane/EtOAc 3:7 to 1:1]