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
30 g 7-methoxy-1-naphthaleneacetamide, 120 ml THF and 35.7 g triethylamine were added into reaction flask. The mixture was stirred and cooled with external ice saline bath. Trifluoroacetic anhydride was slowly added in drops. After completion of addition, it was stirred for further 15 min. Then, the ice bath was removed and stirring was carried out for 2 h at room temperature. After completion of the reaction, the reaction solution was evaporated. Subsequently, 200 ml water was added and the solution was filtered and dried after stirring for 0.5 hours, to obtain 28 g crude product. Recrystallization was carried out using 280 ml isopropyl ether and 1.4 g activated carbon to obtain 22 g refined product with the mp of 82-84° C. The yield is 80%.
WORKUP
后处理
- temperaturecooled with external ice
- additionAfter completion of addition, it
- stirringwas stirred for further 15 min
- customThen, the ice bath was removed
- stirringstirring
- customAfter completion of the reaction
- customthe reaction solution was evaporated
- additionSubsequently, 200 ml water was added
- filtrationthe solution was filtered
- customdried
- stirringafter stirring for 0.5 hours