反应 #3562010
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04035363
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 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. The mixture is heated on reflux for 3 hours 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
来源 ID: ord-9ebb803258dd412bb2171ee05ddcde09