HRID1033009

反应详情

EQUATION

反应方程式

HRID 1033009 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

3[(Benzoxazol-2-yl)methoxy]-2-methoxy-5-ethyl-6-methylpyridine (140 mg, 0.47 mmol) was dissolved in methylene chloride (5 ml) and cooled in an ice bath under an atmosphere of nitrogen. 1M Boron tribomide (2.3 mL, 2.3 mmol) in hexane was added to this solution and the reaction mixture was allowed to warm to room temperature over a 0.75 hour period. This mixture was re-cooled in an ice bath and saturated aqueous NaHCO3 (5 mL) was added to quench the reaction. The methylene chloride layer was dried (Na2SO4), filtered and evaporated. The residue was triturated with diethyl ether to give 69 mg of crude product. Recrystallization from methanol yielded 60 mg (45%), m.p. 198°-200° C.

WORKUP

后处理

  1. temperaturecooled in an ice bath under an atmosphere of nitrogen
  2. temperatureThis mixture was re-cooled in an ice bath
  3. customto quench
  4. customthe reaction
  5. dry with materialThe methylene chloride layer was dried (Na2SO4)
  6. filtrationfiltered
  7. customevaporated
  8. customThe residue was triturated with diethyl ether