反应 #94727

ord-ae7381d00f9e449496d9db8802d2fc34

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他evaporated to dryness
  2. 2
    workup.ADDITIONthe residue is mixed with 30 ml of water and enough 10% sodium hydroxide
  3. 3
    过滤This mixture is filtered
  4. 4
    workup.ADDITIONthe filtrate adjusted to pH 7 by the addition of 10% hydrochloric acid
  5. 5
    其他to precipitate
  6. 6
    过滤The desired compound is filtered off
  7. 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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04342587uspto-grants-1982_08