Реакция #1005947

ord-287538803f06481ea775b8ec999614cc

Уравнение реакции

CCOC(=O)c1cnc(Cl)nc1C(F)(F)F
Ethyl 2-chloro-4-(trifluoromethyl)pyrimidine-5-carboxylate
FC(F)(F)C1(c2cc(Cl)c(Cl)c(Cl)c2)CCNC1
3-(3,4,5-trichlorophenyl)-3-(trifluoromethyl)pyrrolidine
O=C([O-])[O-].[K+].[K+]
potassium carbonate
CCOC(=O)c1cnc(N2CCC(c3cc(Cl)c(Cl)c(Cl)c3)(C(F)(F)F)C2)nc1C(F)(F)F
title compound
Выход 95.0%
CCOC(=O)c1cnc(N2CCC(c3cc(Cl)c(Cl)c(Cl)c3)(C(F)(F)F)C2)nc1C(F)(F)F
ethyl 2-[3-(3,4,5-trichlorophenyl)-3-(trifluoromethyl)-pyrrolidin-1-yl]-4-(trifluoromethyl)pyrimidine-5-carboxylate
Выход 95.0%

Растворители

Условия реакции

Температура
100°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураAfter cooling
  2. 2
    Экстракцияextracted with ethyl acetate
  3. 3
    СушкаThe organic layer was dried over magnesium sulfate
  4. 4
    ДругоеThe solvent was evaporated off under reduced pressure
  5. 5
    Другоеthe residue was then purified by a silica gel chromatography

Методика

Ethyl 2-chloro-4-(trifluoromethyl)pyrimidine-5-carboxylate (1.2 g) [see J. Med. Chem., 43, 3995 (2000)], 3-(3,4,5-trichlorophenyl)-3-(trifluoromethyl)pyrrolidine (1.5 g), and potassium carbonate (0.7 g) were added to N,N-dimethylformamide (50 mL) and the mixture was heated at 100° C. for 5 hours. After cooling, the reaction solution was poured over ice water, and then extracted with ethyl acetate. The organic layer was dried over magnesium sulfate. The solvent was evaporated off under reduced pressure, and the residue was then purified by a silica gel chromatography to obtain the title compound (2.4 g, 95%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09271499B2uspto-grants-2016_03