HRID1769089
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
3.7 g (59 mmol) of ammonium formate and then 0.9 g of 10% palladium-on-charcoal are added to a solution of 0.78 g (2.9 mmol) of 1-(1-propen-2-yl)-5-(1,1-dimethylethoxy)carbonyl-5,6-dihydro-4H-thieno[3, 4-c]pyrrole in 40 ml of methanol. The reaction mixture is heated at reflux for 8 hours, then filtered on a Celite column and evaporated to dryness. The residue is taken up in 50 ml of ethyl acetate, washed with 20 ml of water, dried over sodium sulphate and evaporated to dryness. After purification on a silica column using the 1/4 ethyl acetate/hexane eluent mixture, 0.49 g of an oily product is obtained. Yield 63%.
WORKUP
后处理
- temperatureThe reaction mixture is heated
- temperatureat reflux for 8 hours
- filtrationfiltered on a Celite column
- customevaporated to dryness
- washwashed with 20 ml of water
- dry with materialdried over sodium sulphate
- customevaporated to dryness
- customAfter purification on a silica column