HRID560290
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 mixture of 5-methyl-2-aminothiazole (7.09 mmol) and 2-bromo-3-oxo-butyric acid ethyl ester (8.51 mmol) in acetone (17 mL) is stirred for 16 h at RT and for additional 7 h at reflux. The solvents are removed in vacuo, chloroform and sat aq. NaHCO3 solution are added, the layers are separated and the aq. layer is extracted with chloroform. The combined organic layers are dried over MgSO4 and concentrated in vacuo to give a crude product which is purified by FC (heptane to heptane/EtOAc 6/4). LC-MS: tR=0.80 min; [M+H]+=225.3.
WORKUP
后处理
- temperatureat reflux
- customThe solvents are removed in vacuo, chloroform
- additionare added
- customthe layers are separated
- extractionthe aq. layer is extracted with chloroform
- dry with materialThe combined organic layers are dried over MgSO4
- concentrationconcentrated in vacuo