HRID465948

反应详情

EQUATION

反应方程式

HRID 465948 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a solution of 3-hydroxy-2,2-diethyl-1-propanesulfonamide (1.0 g) in DMF (70 ml) was added sodium hydride (0.45 g), followed by heating at 70° C. for 30 minutes. The mixture to which 6-chloroimidazo [1,2-b]pyridazine (0.8 g) was added was heated for 5 hours. The reaction mixture was cooled, adjusted to pH 6.0 with 1N-hydrochloric acid and then concentrated. The residue was subjected to a silica gel column chlomatography, eluting with chloroform-methanol (10:1). The corresponding combined fractions were concentrated, thereby affording the above-identified compound (1.0 g).

WORKUP

后处理

  1. temperaturewas heated for 5 hours
  2. temperatureThe reaction mixture was cooled
  3. concentrationconcentrated
  4. washeluting with chloroform-methanol (10:1)
  5. concentrationThe corresponding combined fractions were concentrated