反应详情

To a mixture of 1-nitrosopiperazine {1.21 g) and pyridine (2.4 ml) in dioxane (18 ml) was added dropwise 2-thenoyl chloride (1.2 ml) in an ice bath. The mixture was stirred for one hour in an ice.bath and then overnight at ambient temperature. The mixture was poured into a mixture of ethyl acetate (100 ml) and water (100 ml). The separated aqueous layer was extracted twice with ethyl acetate. The combined organic layers were dried and concentrated in vacuo. The residue was pulverized with diisopropyl ether to yield 1-nitroso-4-(2-thenoyl)-piperazine (1.78 g).

1. customovernight
2. customat ambient temperature
3. extractionThe separated aqueous layer was extracted twice with ethyl acetate
4. customThe combined organic layers were dried
5. concentrationconcentrated in vacuo