Reaction #2880884
Related Literature (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04886546
Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
Procedure: A mixture of 2.12 g (10 m mol) of p-chloroacetoacetanilide, 1.07 g (10 m mol) of benzylamine and 20 ml of toluene was refluxed for 1 hour, while the resulted water together with about 12 ml of toluene were distilled off outside the reaction system. After the remaining solvent in the mixture was removed by a rotary evaporator under vacuo, 4.49 g (22 m mol) of 2,2-dimethyl-6-phenyl-4H-1,3-dioxin-4-one, 4.65 g (40 m mol) of N,N,N',N'-tetramethylethylenediamine and 20 ml of xylene were added to the residue. While further refluxing gently for 1.5 hours, the resulted acetone was removed to outside the reaction system. The mixture was cooled to precipitate the crystals. The crystals were filtered and dried to afford 2.63 g of the title compound (yield: 77.5%). were distilled off outside the reaction system After the remaining solvent in the mixture was removed by a rotary evaporator under vacuo, 4.49 g (22 m mol) of 2,2-dimethyl-6-phenyl-4H-1,3-dioxin-4-one, 4.65 g (40 m mol) of N,N,N',N'-tetramethylethylenediamine and 20 ml of xylene were added to the residue While further refluxing gently for 1.5 hours the resulted acetone was removed to outside the reaction system The mixture was cooled to precipitate the crystals The crystals were filtered dried
Source ID: ord-d00000d9f3b745b6a8467c6d78e552d5