反应详情

A solution of 466 mg (1 mmol) of N-[4-(4-Bromo-butoxy)-phenyl]-N-methyl-4-trifluoromethyl-benzenesulfonamide 69-9844 in 3.5 ml DMA was treated at 0° C. with 0.195 ml (2 mmol) of 2-ethylaminoethanol and stirred at RT for 15 h. The reaction mixture was cooled (0° C.) again, treated with 0.195 ml (2 mmol) of 2-ethylaminoethanol and stirred at RT for further 24 h. The solution was concentrated, the residual oil was dissolved in water/acetontrile 1:1/5% formic acid and purified by prep. HPLC: RP-18, acetonitrile/water, 10%-60% acetonitrile. The pure fractions were collected, dissolved in EtOAc, washed with aqueous sat. NaHCO3 solution, and the organic phase was dried (Na2SO4) and evaporated to yield 360 mg (76%) of N-(4-{4-[Ethyl-(2-hydroxy-ethyl)-amino]-butoxy}-phenyl)-N-methyl-4-trifluoromethyl-benzenesulfonamide, MS: 475 (MH+).

1. temperatureThe reaction mixture was cooled (0° C.) again
2. stirringstirred at RT for further 24 h
3. concentrationThe solution was concentrated
4. dissolutionthe residual oil was dissolved in water/
5. custom1/5% formic acid and purified by prep
6. customThe pure fractions were collected
7. dissolutiondissolved in EtOAc
8. washwashed with aqueous sat. NaHCO3 solution
9. dry with materialthe organic phase was dried (Na2SO4)
10. customevaporated