HRID972321

反应详情

EQUATION

反应方程式

HRID 972321 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe reaction mixture was evaporated down at reduced pressure
  2. customthe residue was partitioned between ether and water
  3. dry with materialThe organic phase was dried over anhydrous sodium sulfate
  4. customevaporated at reduced pressure
  5. customto obtain yellow crystals
  6. customRecrystallization from methanol/water
  7. customgave the product (990 mg.), m.p. 99°-100° C.