HRID1584345
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 methyl 2-bromo-3-[3-fluoro-4-(5-methyl-2-phenyl-4-oxazolylmethoxy)phenyl]propionate (14.1 g), 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU) (4.8 g) and toluene (150 ml) was stirred for 2 hours at temperatures ranging from 80 to 90° C. The reaction mixture was poured into 2N HCl, which was subjected to extraction with ethyl acetate. The ethyl acetate layer was washed with water and dried (MgSO4), followed by distilling off the solvent under reduced pressure to yield methyl 3-fluoro-4-(5-methyl-2-phenyl-4-oxazolylmethoxy)cinnamate (10.0 g). The product was recrystallized from dichloromethane-methanol to give colorless prisms, m.p.167-168° C.
WORKUP
后处理
- customranging from 80 to 90° C
- extractionwas subjected to extraction with ethyl acetate
- washThe ethyl acetate layer was washed with water
- dry with materialdried (MgSO4)
- distillationby distilling off the solvent under reduced pressure