HRID903086

反应详情

EQUATION

反应方程式

HRID 903086 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N(1,3-Dimethyl-5-pyrazolyl)-5-methyl isothiourea hydroiodide (Example XXV) (20.0 g) and 11.5 g. -N-methyl ethylenediamine were heated to 120° for 30 minutes and to 160° for 1 hour. After cooling, methylene chloride was added and the solid which formed was filtered and discarded. The methylene chloride solution was shaken with 15% KOH solution, dried over potassium carbonate, concentrated and the residue crystallized from acetonitrile to get 10.16 g. product, mp. 128°-130°.

WORKUP

后处理

  1. temperatureAfter cooling
  2. customthe solid which formed
  3. filtrationwas filtered
  4. dry with materialdried over potassium carbonate
  5. concentrationconcentrated
  6. customthe residue crystallized from acetonitrile
  7. customto get 10.16 g