反应详情

To 15 ml. of dioxane are added 3 g. of ortho-normalpropoxyphenol, 9 ml. of 37% of formalin and 2.4 g. of phenethylamine. The mixture is heated on reflux for 3 hours and distilled to remove the solvent under reduced pressure. The residue is purified by column chromatography on silica gel with a mixture of acetone and benzene (1:4). The resultant oily substance is cooled to be crystallized. A small portion of ethanol is added to the crystals, followed by filtration. The procedure yields 3-phenethyl-8-normal-propoxy-3,4-dihydro-2H-1,3-benzoxazine as colorless needless melting at 84° C. Yield: 3.8 g.

1. temperatureThe mixture is heated
2. temperatureon reflux for 3 hours
3. distillationdistilled
4. customto remove the solvent under reduced pressure
5. customThe residue is purified by column chromatography on silica gel with a mixture of acetone and benzene (1:4)
6. temperatureThe resultant oily substance is cooled
7. customto be crystallized
8. additionA small portion of ethanol is added to the crystals
9. filtrationfollowed by filtration