反应详情

温度

0 °C

To a solution of 2azidomethyl-1,4-dibenzyl-piperazine (9.0 g, 0.028 mol) in TBFE (90 mL) and water (5 mL) was added triphenylphosphine (22.3 g, 0.085 mol) and the mixture stirred for 18 h. The reaction was concentrated to an oil, dissolved in 1N hydrochloric acid (100 mL) and washed with ethyl acetate (2×100 mL). The acidic aqueous layer was cooled to 0° C. and the pH adjusted to 8.5 with 3N sodium hydroxide. The mixture was extracted with ethyl acetate (2×100 mL) and extracts dried over sodium sulfate and concentrated to an oil.

1. concentrationThe reaction was concentrated to an oil
2. dissolutiondissolved in 1N hydrochloric acid (100 mL)
3. washwashed with ethyl acetate (2×100 mL)
4. extractionThe mixture was extracted with ethyl acetate (2×100 mL)
5. dry with materialextracts dried over sodium sulfate
6. concentrationconcentrated to an oil