反应详情

温度

100 °C

A mixture of t-butyl 1-homopiperazine carboxylate (45 mmol, 9 g) and DMF (50 ml) was heated to 100° C. 3,4-dichloro-1,2,5-thiadiazole (23 mmol, 2.2 ml) was added to the mixture and stirred at 100° C. for 2 days. The mixture was quenched with ice/water and extracted with ethyl acetate (3×). The combined organic layer was washed with water (2×) and brine, dried over sodium sulfate, filtered and concentrated. The crude was purified on silica column using 20% ethyl acetate/hexanes to give 5.8 g of product.

1. customThe mixture was quenched with ice/water
2. extractionextracted with ethyl acetate (3×)
3. washThe combined organic layer was washed with water (2×) and brine
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customThe crude was purified on silica column