反应 #94727
ord-ae7381d00f9e449496d9db8802d2fc34
反应方程式
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1其他evaporated to dryness
- 2workup.ADDITIONthe residue is mixed with 30 ml of water and enough 10% sodium hydroxide
- 3过滤This mixture is filtered
- 4workup.ADDITIONthe filtrate adjusted to pH 7 by the addition of 10% hydrochloric acid
- 5其他to precipitate
- 6过滤The desired compound is filtered off
- 7其他dried
实验过程
To a stirred suspension of 1.4 g of 2-amino-5-chloro-5,6-dimethylpyrimidine in 20 ml of dry acetonitrile at room temperature is added 2.2 g of 2-chloropyridine-3-sulfonylisocyanate. The mixture is stirred for several hours, evaporated to dryness and the residue is mixed with 30 ml of water and enough 10% sodium hydroxide to adjust the pH to 11. This mixture is filtered and the filtrate adjusted to pH 7 by the addition of 10% hydrochloric acid and then refiltered. Acidification of this filtrate to pH 2 causes the desired compound to precipitate. The desired compound is filtered off and dried.