HRID1090430

反应详情

EQUATION

反应方程式

HRID 1090430 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

3'-Trimethylgermylacetophenone (49 mg,0.2 mmol) and methyl 4-formylbenzoate (37 mg,0.23 mmol) was dissolved in 5 ml of a mixture of 50% isopropanol and tetrahydrofuran, 1 ml of 1N aqueous potassium hydroxide solution was added, and the mixture was stirred overnight. The reaction mixture was adjusted to pH1 with 2N hydrochloric acid and extracted with AcOEt. The extract was evaporated and the residue was purified by column chromatography on silica gel (eluent: MeOH-methylene chloride) and recrystallized from a mixture of AcOEt and n-hexane to give 17 mg of pale yellow prisms, m.p.186°-188° C. (yield 22%).

WORKUP

后处理

  1. additionwas added
  2. extractionextracted with AcOEt
  3. customThe extract was evaporated
  4. customthe residue was purified by column chromatography on silica gel (eluent: MeOH-methylene chloride)
  5. customrecrystallized from a mixture of AcOEt and n-hexane