反应详情

Compound 72B (9.12 g, 44.4 mmol) was dissolved in 50 ml DMF. NaH was added portionwise over 5 minutes. After stirring for 15 minutes a solution of thiocarbamoyl chloride (5.8 g, 46.7 mmol) in 25 ml DMF was added and allowed to stir for 2 h. 50 ml 2N HCl was added and the reaction was extracted 2×100 ml ether, washed 2×100 ml water, 1×100 ml brine, and filtered through silica. The product was eluted with 200 ml diethyl ether and concentrated. The precipitate was filtered and dried under vacuum for 16 h. MS m/z 293 (M+1).

1. additionwas added
2. extractionthe reaction was extracted 2×100 ml ether
3. washwashed 2×100 ml water, 1×100 ml brine
4. filtrationfiltered through silica
5. washThe product was eluted with 200 ml diethyl ether
6. concentrationconcentrated
7. filtrationThe precipitate was filtered
8. customdried under vacuum for 16 h