反应详情

温度

4 °C

Sodium nitrite (0.33 g) in water (20 ml) was added over 15 minutes to a solution of 3-amino-2-[4-(5-bromo-3-methylpyrid-2-yl)butylamino]-5-(pyrid-3-ylmethyl)pyridine (2.0 g) in molar sulphuric acid (100 ml) stirred at 4° C. The solution was then allowed to warm to room temperature, basified with concentrated ammonium hydroxide solution and extracted with chloroform (3 x 100 ml). The chloroform extracts were combined, dried over magnesium sulphate, and the solvent removed to give a product which was recrystallised from acetonitrile to give the title compound (1.49 g) as prims, m.p. 114°-115° C.

1. temperatureto warm to room temperature
2. extractionextracted with chloroform (3 x 100 ml)
3. dry with materialdried over magnesium sulphate
4. customthe solvent removed
5. customto give a product which
6. customwas recrystallised from acetonitrile