反应详情

A suspension of 21.9 g of 5-(2-aminoethoxy)-salicylamide, 36.0 g of α-(bromomethyl)-benzyl alcohol and 30 g of potassium bicarbonate in 240 ml of ethanol is refluxed for 15 hours, with stirring. The reaction mixture is then cooled and filtered and the filtrate is evaporated. The evaporation residue is partitioned between 300 ml of ethyl acetate and 100 ml of water and the organic phase is separated off, dried over magnesium sulfate and evaporated. The residue is dissolved hot in as little ethanol as possible and made to crystallise, yielding α-[N-[2-(3-carbamoyl-4-hydroxy-phenoxy)ethyl]-aminomethyl]-benzyl alcohol with a melting point of 174°-175° (from ethanol).

1. temperatureis refluxed for 15 hours
2. temperatureThe reaction mixture is then cooled
3. filtrationfiltered
4. customthe filtrate is evaporated
5. customThe evaporation residue is partitioned between 300 ml of ethyl acetate and 100 ml of water
6. customthe organic phase is separated off
7. dry with materialdried over magnesium sulfate
8. customevaporated
9. dissolutionThe residue is dissolved hot in as little ethanol as possible and
10. customto crystallise