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
3. addition1)was 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