HRID1914872

反应详情

EQUATION

反应方程式

HRID 1914872 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6,7-Difluoro-1-(2-fluoro-4-iodo-phenyl)-4-methoxy-1,3-dihydro-benzoimidazol-2-one (3.0 g, 7.14 mmol) was added portion wise to fuming nitric acid at −78° C. over a period of 1 minute and the resulting mixture was stirred at room temperature for 5 minutes. The reaction was monitored by TLC (50% ethyl acetate in hexane). The reaction mixture was quenched with cold water. The solid formed was collected, washed with water and dried to give the crude product. Purification by column chromatography on silica gel (10-40% ethyl acetate in hexane) afforded 1.6 g of the product (48.2% yield).

WORKUP

后处理

  1. customThe reaction mixture was quenched with cold water
  2. customThe solid formed
  3. customwas collected
  4. washwashed with water
  5. customdried
  6. customto give the crude product
  7. customPurification by column chromatography on silica gel (10-40% ethyl acetate in hexane)