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
To a suspension of 4-(2-Ethyl-imidazo[4,5-c]quinolin-1-yl)-butylamine obtained in step VI in tetrahydrofuran was added acetic acid (1 eq.) and dihydrothiophen-3-one (1.1 eq.). Resulting reaction mixture was stirred for 10 min. Sodium triacetoxyborohydride (2.2 eq.) was added to reaction mixture over a period of 1 hrs and resulting suspension was then stirred for 4-5 hrs. Reaction was then quenched with methanol and concentrated to dryness. Reaction mixture was basified using aq.sodium hydroxide solution and extracted with chloroform. Organic layer was dried over sodium sulphate and concentrated under reduced pressure to yield sticky solid. Product was then purified by silica gel column chromatography to afford [4-(2-Ethyl-imidazo[4,5-c]quinolin-1-yl)-butyl]-(tetrahydro-thiophen-3-yl)-amine.
WORKUP
后处理
- customResulting
- customreaction mixture
- customresulting suspension
- stirringwas then stirred for 4-5 hrs
- customReaction
- customwas then quenched with methanol
- concentrationconcentrated to dryness
- customReaction mixture
- extractionsodium hydroxide solution and extracted with chloroform
- dry with materialOrganic layer was dried over sodium sulphate
- concentrationconcentrated under reduced pressure
- customto yield sticky solid
- customProduct was then purified by silica gel column chromatography