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
0.32 g (1.00 mmol) 4-Chloromethyl-2-[2-(4-trifluoromethylsulfanyl-phenyl)-vinyl]-oxazole, 0.217 g (1.00 mmol) 4-(4-[1,2,3]Triazol-1-yl-butyl)-phenol, 0.166 g (1.00 mmol) potassium iodide and 0.191 ml (1.00 mmol) of sodium methylate (30% in methanol) were added to 50.0 ml methanol and heated to reflux for 16 h. After removal of solvent and partitioning of the residue between 50 ml ethyl acetate and 15 ml water, the organic phase was washed with 10 ml water, 10 ml 0.1 N NaOH and twice 15 ml water, and dried over sodium sulfate. The solution was concentrated until crystallisation of the product started. After leaving for 1 h at room temperature the precipitate was isolated, washed with ether and dried at 40° C. in vacuo. Yield 0.11 g (18%) 1-[4-(4-{2-[2-(4-Trifluoromethylsulfanyl-phenyl)-vinyl]-oxazol-4-ylmethoxy}-phenyl)-butyl]-1H-[1,2,3]triazole, m.p. 144–145° C.
WORKUP
后处理
- temperatureheated
- temperatureto reflux for 16 h
- customAfter removal of solvent
- custompartitioning of the residue between 50 ml ethyl acetate and 15 ml water
- washthe organic phase was washed with 10 ml water, 10 ml 0.1 N NaOH and twice 15 ml water
- dry with materialdried over sodium sulfate
- concentrationThe solution was concentrated until crystallisation of the product
- customAfter leaving for 1 h at room temperature the precipitate
- customwas isolated
- washwashed with ether
- customdried at 40° C. in vacuo