HRID1584477
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- extractionExtract with a saturated aqueous solution of sodium bicarbonate
- dry with materialdry over Na2SO4
- filtrationfilter
- customevaporate in vacuo
- customto give a residue
- temperatureCool in an ice bath
- customevaporate
- customto remove most of the methanol
- customtriturate with diethyl ether (150 mL)
- customto give a solid
- customDecant the solvent
- additionadd diethyl ether (150 mL)
- customcollect the solid
- filtrationby filtration
- customto give
- customafter drying