Reaction #477873

ord-6e2037cd9b214b8abc18800156358393

Conditions

Temperature
100°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    OtherThe residue is purified by chromatography on a column of silica
  2. 2
    Washeluted with a 70/30 heptane/ethyl acetate mixture

Procedure

172 μL (1 mmol) of heptyl isocyanate are added to 251 mg (0.8 mmol) of ethyl 2-[1-(3′-methylaminobiphenyl-4-yl)meth-(E)-ylidene]pentanoate (prepared according to Example 8a). The reaction mixture is heated at 100° C. in an Emrys Optimizer microwave oven for 20 minutes. The residue is purified by chromatography on a column of silica eluted with a 70/30 heptane/ethyl acetate mixture. 361 mg (100%) of ethyl 2-[1-[3′-(3-heptyl-1-methylureido)biphenyl-4-yl]meth-(E)-ylidene]pentanoate are obtained in the form of a yellowish oil.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08383652B2uspto-grants-2013_02