反应详情

温度

0 °C

A mixture of 24.6 grams (0.15 mole) of N,N-dimethyl-N'-phenyl-ethylenediamine and 18.2 grams (0.18 mole) of triethylamine in 500 milliliters of tetrahydrofuran (THF) is cooled to 0° C. and 39.8 grams (0.18 mole) of 5-methyl-3-phenyl-4-isoxazole carbonyl chloride in 100 milliliters of tetrahydrofuran is added dropwise. After the addition is complete, the mixture is warmed to room temperature and stirred for 4 hours. The resulting suspension is filtered and the THF removed in vacuo. The residue is dissolved in methylene chloride and washed with 2N sodium hydroxide and water and then dried over magnesium sulfate. The mixture is filtered and the solvent removed by evaporation. The residue is then treated with hexane to yield crystals of N-phenyl-N-(2-dimethylaminoethyl)-5-methyl-3-phenyl-4-isoxazole carboxamide; M.P. 88°-89° C.

1. additionAfter the addition
2. temperaturethe mixture is warmed to room temperature
3. filtrationThe resulting suspension is filtered
4. customthe THF removed in vacuo
5. dissolutionThe residue is dissolved in methylene chloride
6. washwashed with 2N sodium hydroxide and water
7. dry with materialdried over magnesium sulfate
8. filtrationThe mixture is filtered
9. customthe solvent removed by evaporation
10. additionThe residue is then treated with hexane