反应详情

温度

100 °C

A suspension of 6 g (0.0205 mol) of 4-tert-butyloxycarbonyl-1-(4-hydroxyphenyl)-2-methylpiperazine, 2.4 ml (0.0246 mol) of methyl bromoacetate and 3.4 g (0.0246 mol) of potassium carbonate in 50 ml of dimethylformamide is heated at 100° C. for 6 hours and, after cooling, concentrated to dryness in vacuo. The residue is partitioned between ethyl acetate and water and the aqueous phase is extracted once more with ethyl acetate. The combined ethyl acetate extracts are concentrated to dryness in vacuo. The residue is purified by means of chromatography on a silica gel column, ethyl acetate/cyclohexane being used as eluent. After evaporation, the residue is crystallized from ether/petroleum ether.

1. temperatureafter cooling
2. concentrationconcentrated to dryness in vacuo
3. customThe residue is partitioned between ethyl acetate and water
4. extractionthe aqueous phase is extracted once more with ethyl acetate
5. concentrationThe combined ethyl acetate extracts are concentrated to dryness in vacuo
6. customThe residue is purified by means of chromatography on a silica gel column, ethyl acetate/cyclohexane being
7. customAfter evaporation
8. customthe residue is crystallized from ether/petroleum ether