HRID442723

反应详情

EQUATION

反应方程式

HRID 442723 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-(3-bromo-4-fluorobenzoyl)-3-methoxymethoxypyridine (4.68 g) in dimethyl sulfoxide (50 mL) was added potassium cyanide (2.7 g) at 0° C. The mixture was stirred for 3 hours while raising the temperature to room temperature. The reaction mixture was poured into water, which was subjected to extraction with ethyl acetate. The extract solution was washed with water and a saturated aqueous saline solution, successively, and dried (sodium sulfate) and then concentrated. The concentrate was purified by means of a silica gel column (ethyl acetate--hexane) to afford 2-(3-bromo-4-cyanobenzoyl)-3-methoxymethoxypyridine (4.59 g) (compound B-6). Physical properties and spectrum date of the product are shown in Table 3 and Table 4.

WORKUP

后处理

  1. extractionwas subjected to extraction with ethyl acetate
  2. washThe extract solution was washed with water
  3. dry with materiala saturated aqueous saline solution, successively, and dried (sodium sulfate)
  4. concentrationconcentrated
  5. customThe concentrate was purified by means of a silica gel column (ethyl acetate--hexane)