HRID543056

反应详情

EQUATION

反应方程式

HRID 543056 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

22.8 parts of 1,4-diaminoanthraquinone-2-sulfonic acid (78.1%) are added at room temperature to a mixture of 53 parts of 2-pyrrolidone and 52 parts of water. The pH of the solution is adjusted to 7.5-8 with 5 parts of 24% aqueous ammonia solution. Then 2 parts of ammonium bicarbonate, 6.4 parts of 3-nitrobenzene-1-sulfonic acid, sodium salt, and 9 parts of sodium cyanide are added in succession. The reaction mixture is then heated for 4 hours to 88° C., with stirring. The precipitate is filtered warm with suction, washed with warm 25% aqueous 2-pyrrolidone and then with hot water, and dried at 50° C. in vacuo, affording 14.9 parts of 95.5% 1,4-diamino-2,3-dicyanoanthraquinone, corresponding to a yield of 88.3% of theory. Rf =0.54.

WORKUP

后处理

  1. temperatureThe reaction mixture is then heated for 4 hours to 88° C.
  2. filtrationThe precipitate is filtered
  3. temperaturewarm with suction
  4. washwashed
  5. temperaturewith warm 25% aqueous 2-pyrrolidone
  6. dry with materialwith hot water, and dried at 50° C. in vacuo