HRID1253031

反应详情

EQUATION

反应方程式

HRID 1253031 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
23 °C

PROCEDURE

实验过程

Dry, powdered sodium cyanide (14 gm, 280 mmole) was added to 80 ml of dry dimethylsulfoxide with stirring at 23° C. Then 1-benzyl-2-chloromethylimidazole hydrochloride (14 gm, 63 mmole) was added portionwise over 10 minutes while maintaining the temperature below 40° C. After the addition was complete, the mixture was stirred at 40° C. for an additional hour. It was diluted with 250 ml methylene chloride and the resulting solution was washed with 4×200 ml of water, dried over MgSO4 and the solvent removed in vacuo. The residue was collected by filtration, dissolved in warm methanol and precipitated with ether to obtain needle-like crystals (8.7 g) of N-benzyl-2-cyanomethylimidazole. m.p. 102.5°-104° C.

WORKUP

后处理

  1. customDry
  2. temperaturewhile maintaining the temperature below 40° C
  3. additionAfter the addition
  4. stirringthe mixture was stirred at 40° C. for an additional hour
  5. washthe resulting solution was washed with 4×200 ml of water
  6. dry with materialdried over MgSO4
  7. customthe solvent removed in vacuo
  8. filtrationThe residue was collected by filtration
  9. dissolutiondissolved in warm methanol
  10. customprecipitated with ether