HRID615444

反应详情

EQUATION

反应方程式

HRID 615444 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

6-Methoxybenzothiazol-2-ylguanidine (0.2 g) was added to a suspension of sodium hydride (0.022 g=0.044 g of 50% dispersion in oil) in anhydrous dimethylformamide (20 mls) and the resulting mixture was stirred at room temperature for 15 mins. 4-(2-Diethylaminoethoxy)phenylisothiocyanate (0.23 g) was added followed, after 2.5 hrs, by methyl iodide (0.14 g) and the mixture stirred for a further 18 hrs. Water was added to precipitate a yellow solid which was collected by filtration, washed with ethanol and dissolved in ethyl acetate. The ethyl acetate solution was dried over anhydrous sodium sulphate and evaporated to give a yellow solid (0.33 g). Recrystallisation of the residue from ethyl acetate gave the desired product as pale yellow crystals (0.08 g) mp 189.5°-191°.

WORKUP

后处理

  1. stirringthe mixture stirred for a further 18 hrs
  2. customto precipitate a yellow solid which
  3. filtrationwas collected by filtration
  4. washwashed with ethanol
  5. dissolutiondissolved in ethyl acetate
  6. dry with materialThe ethyl acetate solution was dried over anhydrous sodium sulphate
  7. customevaporated