HRID1584477

反应详情

EQUATION

反应方程式

HRID 1584477 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Combine 4-(1-(fur-2-ylmethyl)-1H-benzimidazol-2-yl)[1,4]diazepane hydrochloric acid salt (0.57 g, 1.53 mmol) and dichloromethane (150 mL). Extract with a saturated aqueous solution of sodium bicarbonate, dry over Na2SO4, filter, and evaporate in vacuo to give a residue. Combine the residue and methanol (50 mL). Cool in an ice bath. Add aqueous hydriodic acid (0.194 g, 57%, 1.52 mmol). After 30 minutes, evaporate to remove most of the methanol and triturate with diethyl ether (150 mL) to give a solid. Decant the solvent, add diethyl ether (150 mL) and collect the solid by filtration to give, after drying, the title compound.

WORKUP

后处理

  1. extractionExtract with a saturated aqueous solution of sodium bicarbonate
  2. dry with materialdry over Na2SO4
  3. filtrationfilter
  4. customevaporate in vacuo
  5. customto give a residue
  6. temperatureCool in an ice bath
  7. customevaporate
  8. customto remove most of the methanol
  9. customtriturate with diethyl ether (150 mL)
  10. customto give a solid
  11. customDecant the solvent
  12. additionadd diethyl ether (150 mL)
  13. customcollect the solid
  14. filtrationby filtration
  15. customto give
  16. customafter drying