HRID637083

反应详情

EQUATION

反应方程式

HRID 637083 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Combine 1-(t-butoxycarbonyl)-4-(1-(2-cyanomethyloxyethyl)-1H-benzimidazol-2-yl)[1,4]diazepane (0.36 g, 0.91 mmol), dichloromethane (15 mL), and methanol (5 mL). Cool in an ice bath and add hydriodic acid (0.25 mL, 57%, 1.86 mmol). Warm to ambient temperature. After 5 hours, concentrate the reaction mixture in vacuo to give a residue. Combine the residue and diethyl ether (40 mL) and stir. After 18 hours, decant the solvent, add diethyl ether, and stir to give a solid. Collect the solid by filtration and dry to give the title compound.

WORKUP

后处理

  1. temperatureCool in an ice bath
  2. concentrationconcentrate the reaction mixture in vacuo
  3. customto give a residue
  4. waitAfter 18 hours
  5. customdecant the solvent
  6. additionadd diethyl ether
  7. stirringstir
  8. customto give a solid
  9. customCollect the solid
  10. filtrationby filtration
  11. customdry