反应详情

Ten grams (0.035 mol) of 1-(2-cyano-4-n-hexanoylamino-phenoxy)-2,3-epoxypropane were dissolved in 100 ml of ethanol, 7.3 gm (0.1 mol) of sec.butylamine were added, and the mixture was refluxed for one hour. After the solvent was distilled off in vacuo, the residue was purified by column chromatography in the manner described in Example 6. The base thus obtained was dissolved in ethyl acetate, washed with dilute NaOH and water, dried, and evaporated to dryness. The test substance remaining was recrystallized from ethyl acetate with the addition of petroleum ether. Subsequent recrystallization from acetonitrile yielded 2.4 gm of pure white crystalline base. M.p.: 72°-74° C.

1. temperaturethe mixture was refluxed for one hour
2. distillationAfter the solvent was distilled off in vacuo
3. customthe residue was purified by column chromatography in the manner
4. customThe base thus obtained
5. washwashed with dilute NaOH and water
6. customdried
7. customevaporated to dryness
8. customThe test substance remaining was recrystallized from ethyl acetate with the addition of petroleum ether
9. customSubsequent recrystallization from acetonitrile