HRID32509

反应详情

EQUATION

反应方程式

HRID 32509 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Potassium carbonate (3.13 g) was added to 1-methyl-4-phenyl-1H-imidazole-5-carbaldehyde (intermediate 2) (2.33 g) dissolved in acetone (125 mL) and water (25 mL). Once dissolved, potassium permanganate (4.23 g) was added and the mixture stirred for 24 hours. The mixture was filtered through diatomaceous earth and the cake washed with water (2×20 mL). Acetone was evaporated from the filtrate which was extracted with EtOAc (50 mL). The aqueous layer was acidified with acetic acid to pH 5, reduced to half volume and a cream precipitate filtered and dried at 60° C. in vacuo to give the title compound as a cream solid (1.74 g, 69%);

WORKUP

后处理

  1. dissolutionOnce dissolved
  2. filtrationThe mixture was filtered through diatomaceous earth
  3. washthe cake washed with water (2×20 mL)
  4. customAcetone was evaporated from the filtrate which
  5. extractionwas extracted with EtOAc (50 mL)
  6. filtrationa cream precipitate filtered
  7. customdried at 60° C. in vacuo