HRID635171

反应详情

EQUATION

反应方程式

HRID 635171 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.6 g of 1-(2-chloro-5-pyridylmethyl)-3-nitroguanidine and 0.4 g of bis(chloromethyl)methylamine were suspended in dried THF. To the suspension, a solution of 0.52 g of triethylamine in THF was added dropwise with cooling. The reaction mixture was stirred for 1 hour, and then poured into ice water. The mixture was extracted with dichloromethane. After the extract was dried over anhydrous magnesium sulfate, dichloromethane was distilled off. The residue was recrystallized from methanol to obtain 0.78 g of the title compound. This compound is No. 1 in Table 1. m.p.: 150-154° C.

WORKUP

后处理

  1. temperaturewith cooling
  2. extractionThe mixture was extracted with dichloromethane
  3. dry with materialAfter the extract was dried over anhydrous magnesium sulfate, dichloromethane
  4. distillationwas distilled off
  5. customThe residue was recrystallized from methanol