反应详情

A solution of N-nitroso-N'-2-thenylpiperazine (3.0 g, 0.014 mole) in anhydrous freshly distilled tetrahydrofurane (30 ml) was added dropwise to a stirred suspension of lithium aluminium hydride (1.5 g excess) under nitrogen in anhydrous tetrahydrofuran (150 ml) at 60°-65° C. After addition, stirring was continued for 3 hours. Work-up via cooling, controlled addition of water (1.5 ml), 10% sodium hydroxide (2.25 ml) and water (3.75 ml) followed by filtration, drying over potassium carbonate, filtration and evaporation in vacuo gave N-amino-N'-2-thenyl-piperazine (2.7 g, 96%) as an almost colourless oil, used without further purification,

1. additionAfter addition
2. temperatureWork-up via cooling
3. filtrationfollowed by filtration
4. dry with materialdrying over potassium carbonate, filtration and evaporation in vacuo