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
1 mmol of 2-methylthieno[3,4-d][1,3]oxazole was dissolved in 10 ml of tetrahydrofuran and the temperature was kept at −78° C. in a methanol bath cooled by dry ice. A solution in which 1.05 mmol of N-bromosuccinimide was dissolved in 5 ml of tetrahydrofuran was gradually added dropwise to carry out the reaction for 2 hours. Then an excess amount of saturated sodium chloride aqueous solution was added to stop the reaction. The reacted liquid was washed with water. Then the organic layer was recovered and dried under sodium sulfate. The solvent was evaporated out. The product was purified using column separation with the solvent of ethylacetate and hexane, obtaining 6-bromo-2-methylthieno[3,4-d][1,3]oxazole represented by formula (21).
WORKUP
后处理
- customthe temperature was kept at −78° C. in a methanol bath
- additionwas gradually added dropwise
- customthe reaction for 2 hours
- customthe reaction
- washThe reacted liquid was washed with water
- customThen the organic layer was recovered
- customdried under sodium sulfate
- customThe solvent was evaporated out
- customThe product was purified
- customcolumn separation with the solvent of ethylacetate and hexane