HRID1390016

反应详情

EQUATION

反应方程式

HRID 1390016 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The solution of 80 grams of 2-(2-diethylaminoethylamino)-3-amino-6-chloropyridine in 900 ml of dioxane was treated with stirring with 32 ml of pyridine and 36.6 ml of ethyl chloroformate and stirred for one hour. The product precipitating thereby was washed with water and dried (2-(2-diethylaminoethylamino)-3-carbethoxy-amino-6-chloropyridine, M.P. 205°-206° C.) and subsequently melted with occasional stirring and held for 3 hours at 190°-210° C. After cooling the solidified melt was recrystallized from methanol under the addition of activated carbon and isopropanolic H Cl. M.P. of the hydrochloride 252°-254° C.; Yield 52.8 grams.

WORKUP

后处理

  1. customThe product precipitating
  2. washthereby was washed with water
  3. dry with materialdried (2-(2-diethylaminoethylamino)-3-carbethoxy-amino-6-chloropyridine, M.P. 205°-206° C.)
  4. stirringwith occasional stirring
  5. waitheld for 3 hours at 190°-210° C
  6. temperatureAfter cooling the solidified melt
  7. customwas recrystallized from methanol under the addition of activated carbon and isopropanolic H Cl
  8. customM.P. of the hydrochloride 252°-254° C.