HRID1255865

反应详情

EQUATION

反应方程式

HRID 1255865 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 2-nitro-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)aniline (2.35 g, 8.9 mmol) in ethyl acetate (100 mL) was treated with platinum(IV) oxide (0.2 g) and stirred vigorously under a hydrogen atmosphere for 30 minutes. The reaction mixture was degassed with nitrogen and filtered through celite washing with ethyl acetate. This solution was then treated with CDI (1.8 g, 11.1 mmol) and stirred overnight at ambient temperature. The solution was diluted with methylene chloride (100 mL) and the precipate was filtered and washed with cold methanol. The solids were dried in vacuo to yield 5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1,3-dihydro-2H-benzimidazol-2-one as a white solid.

WORKUP

后处理

  1. customThe reaction mixture was degassed with nitrogen
  2. filtrationfiltered
  3. washthrough celite washing with ethyl acetate
  4. stirringstirred overnight at ambient temperature
  5. filtrationthe precipate was filtered
  6. washwashed with cold methanol
  7. customThe solids were dried in vacuo