反应详情

温度

0 °C

4-Bromo-5-isoquinolylsulphonyl chloride may be obtained by the following process: a solution of 5-amino- 4-bromoisoquinoline (4.46 g) in concentrated hydrochloric acid (d=1.19) (44 cc) is cooled to -5° C. then is treated with a solution of sodium nitrite (1.93 g) in water (10 cc). The reaction mixture is stirred for 1 hour at 0° C. The solution obtained is poured into a saturated solution of sulphur dioxide in acetic acid (48 ml), to which has been added a solution of cuprous chloride (0.65 g) in water (5.6 cc). The reaction mixture is stirred until the evolution of gas has finished, and then is extracted with dichloromethane (2×100 cc). The organic phases are pooled, washed with water, dried over magnesium sulphate and concentrated. 4-Bromo-5-isoquino lylsulphonyl chloride (5.6 g) is obtained in the form of a yellow solid which is used as such in the subsequent syntheses.

1. customThe solution obtained
2. stirringThe reaction mixture is stirred until the evolution of gas
3. extractionis extracted with dichloromethane (2×100 cc)
4. washwashed with water
5. dry with materialdried over magnesium sulphate
6. concentrationconcentrated