Реакция #1373

ord-a6bc9092d4d54296b6f4a8701204549f

Уравнение реакции

CCOC=C(C(=O)OCC)C(=O)c1c(F)cc(F)c(F)c1C
Ethyl 2-(2-methyl-3,4,6-trifluorobenzoyl)-3-ethoxyacrylate
NC1CC1
cyclopropylamine
CCOC(=O)C(=CNC1CC1)C(=O)c1c(F)cc(F)c(F)c1C
ethyl 2-(2-methyl-3,4,6-trifluorobenzoyl)-3-cyclopropylaminoacrylate

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураcooling
  2. 2
    Концентрированиеthe mixture is concentrated
  3. 3
    Другоеthe residue is purified with column chromatography (silica-gel, dichloromethane: n-hexane =1: 1)

Методика

Ethyl 2-(2-methyl-3,4,6-trifluorobenzoyl)-3-ethoxyacrylate (3.5 g) is dissolved in ethanol (25 ml) and thereto cyclopropylamine (0.84 ml) is added dropwise under ice-cooling. After stirring at room temperature for 30 minutes, the mixture is concentrated and the residue is purified with column chromatography (silica-gel, dichloromethane: n-hexane =1: 1) to give ethyl 2-(2-methyl-3,4,6-trifluorobenzoyl)-3-cyclopropylaminoacrylate (2.7 g).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05723648uspto-grants-1998_03