反应详情

温度

25 °C

Mix 267 mg (1 mmole) of 3-cyano-dibenzo[b,f]thiepin-5,5-dioxide, 10 ml pyridine, 5 ml acetic acid, and 5 ml water. Add 0.5 g sodium hypophosphite and approximately 0.1 g Raney nickel. Stir at 25° C. for 24 hours and then at 45°-50° C. for 2 hours. Filter the reaction mixture to remove the catalyst and wash any product from the catalyst using 10 ml ethyl acetate. Add 10 ml 6N hydrochloric acid and separate the organic layer containing the product. Evaporate the organic layer to obtain a solid residue comprising the title product, m.p., 175°-177° C. Swishing with methanol and drying the residue gives product melting at 177°-178° C.

1. waitat 45°-50° C. for 2 hours
2. filtrationFilter the reaction mixture
3. customto remove the catalyst
4. washwash any product from the catalyst
5. additionAdd 10 ml 6N hydrochloric acid
6. customseparate the organic layer
7. additioncontaining the product
8. customEvaporate the organic layer
9. customto obtain a solid residue