反应详情

A solution of 6.2 g of 3-tosyloxy-2,2-dimethyl-1-propanesulfonamide and 3.75 g of potassium thiocyanate in 30 ml of dimethylformamide was stirred at 130°-140° C. for 6 hours, and then concentrated to dryness. A mixture of dichloromethane and methanol (9:1) was added to the residue, followed by filtration to remove insoluble material. The filtrate was concentrated and the residue was subjected to a column chromatography, eluting with chloroform-ethyl acetate (2:1). The relevant fractions were concentrated to obtain 0.87 g of 3-thiocyanato-2,2-dimethyl-1-propanesulfonamide as yellow oil.

1. concentrationconcentrated to dryness
2. additionA mixture of dichloromethane and methanol (9:1)
3. additionwas added to the residue
4. filtrationfollowed by filtration
5. customto remove insoluble material
6. concentrationThe filtrate was concentrated
7. washeluting with chloroform-ethyl acetate (2:1)
8. concentrationThe relevant fractions were concentrated