反应详情

温度

50 °C

A mixture of 263 mg (1.45 mmol, 1.2 eq) of C-(5-methylfuran-2-yl)-C-(3-methyloxetan-3-yl)methylamine and 1.02 g (1.21 mmol, 1 eq) of 3-(3H-benzotriazol-4-ylamino)-4-methoxycyclobut-3-ene-1,2-dione at 29% in 25 ml of methanol was heated at 50° C. for 24 hours. The insoluble material (dimer) was filtered off and the filtrate was evaporated. The residue was chromatographed on silica gel (column puriFlash PF-30SIHP/40G, Spot II) eluted with dichloromethane/methanol (gradient). The solid was taken up with ethyl acetate and this organic phase was washed several times with a 1 N sodium dihydrogen phosphate solution, dried over magnesium sulfate, filtered and evaporated. 205 mg of 3-(3H-benzotriazol-4-ylamino)-4-{[(5-methyl furan-2-yl)-(3-methyloxetan-3-yl)methyl]amino}cyclobut-3-ene-1,2-dione were obtained in the form of a yellow solid. (Mp=178-180° C.). Yield=43%, LC/MS: 95.97% [393].

1. filtrationThe insoluble material (dimer) was filtered off
2. customthe filtrate was evaporated
3. customThe residue was chromatographed on silica gel (column puriFlash PF-30SIHP/40G, Spot II)
4. washeluted with dichloromethane/methanol (gradient)
5. washthis organic phase was washed several times with a 1 N sodium dihydrogen phosphate solution
6. dry with materialdried over magnesium sulfate
7. filtrationfiltered
8. customevaporated