HRID502594

反应详情

EQUATION

反应方程式

HRID 502594 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-thioxo-1,2-dihydropyridine-3-carbonitrile (2.1 g, 15.44 mmol) in ethyl acetate (50 mL), bromine (5.9 g, 37.11 mmol) was added drop wise at 0° C. The reaction mixture was allowed to warm to room temperature and then refluxed for 3 h. The reaction mixture was concentrated under reduced pressure. Trituration with hexanes:methylene chloride (1:1) mixture gave 3-bromoisothiazolo[5,4-b]pyridine, as light brown solid which was carried forward without further purification. MW=215 confirmed by LC-MS, tr=16.08 min (Method Y) MH+=216.

WORKUP

后处理

  1. temperaturerefluxed for 3 h
  2. concentrationThe reaction mixture was concentrated under reduced pressure