반응 #52901

ord-7af937a590974f16ad36907baa32ed2e

반응 방정식

COC1=NC(c2cccc(Cl)c2)C(C(=O)NCCC(c2ccccc2)c2ccccc2)=C(C)N1
4-(3-chlorophenyl)-2-methoxyl-6-methyl-1,4-dihydropyrimidine-5-carboxylic acid (3,3-diphenylpropyl)amide
O=C([O-])[O-].[NH4+].[NH4+]
ammonium carbonate
CC(=O)[O-].[NH4+]
ammonium acetate
CC1=C(C(=O)NCCC(c2ccccc2)c2ccccc2)C(c2cccc(Cl)c2)N=C(N)N1
title compound
CC1=C(C(=O)NCCC(c2ccccc2)c2ccccc2)C(c2cccc(Cl)c2)N=C(N)N1
2-amino-4-(3-chlorophenyl)-6-methyl-1,4-dihydropyrimidine-5-carboxylic acid (3,3-diphenylpropyl)amide

반응 조건

온도
80°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타An insoluble matter thus formed
  2. 2
    여과was filtered out
  3. 3
    농축the filtrate was concentrated under reduced pressure
  4. 4
    기타The residue was purified by the basic silica gel chromatography (100% dichloromethane)

실험 절차

111 mg (0.234 mmol) of 4-(3-chlorophenyl)-2-methoxyl-6-methyl-1,4-dihydropyrimidine-5-carboxylic acid (3,3-diphenylpropyl)amide was dissolved in 5 ml of ethanol. 67.4 mg (0.702 mmol) of ammonium carbonate and 11.8 mg (0.187 mmol) of ammonium acetate were added to the obtained solution, and they were stirred at 80° C. for 2 days. The reaction mixture was diluted with ethyl acetate. An insoluble matter thus formed was filtered out, and the filtrate was concentrated under reduced pressure. The residue was purified by the basic silica gel chromatography (100% dichloromethane) to obtain the title compound.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06855716B2uspto-grants-2005_02