HRID972321
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
534 mg. (3 mmol.) of N-bromosuccinimide (recrystallized from water) were added in small portions to a solution of 831 mg. (3 mmol.) of 3-acetyl-2,6-di-t-butylamino-4-methylpyridine (Compound V) in 20 ml. of carbon tetrachloride and 5 ml. of ethanol, and the reaction mixture was allowed to stand overnight at room temperature. The reaction mixture was evaporated down at reduced pressure, and the residue was partitioned between ether and water. The organic phase was dried over anhydrous sodium sulfate and evaporated at reduced pressure to obtain yellow crystals. Recrystallization from methanol/water gave the product (990 mg.), m.p. 99°-100° C.
WORKUP
后处理
- customThe reaction mixture was evaporated down at reduced pressure
- customthe residue was partitioned between ether and water
- dry with materialThe organic phase was dried over anhydrous sodium sulfate
- customevaporated at reduced pressure
- customto obtain yellow crystals
- customRecrystallization from methanol/water
- customgave the product (990 mg.), m.p. 99°-100° C.