反应 #1005948

ord-756c63ce60274dfaaca1bf8dbc209a1e

反应方程式

Cl
hydrochloric acid
[Na+].[OH-]
sodium hydroxide
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
O=C(O)c1cnc(N2CCC(c3cc(Cl)c(Cl)c(Cl)c3)(C(F)(F)F)C2)nc1C(F)(F)F
title compound
收率 92.3%
O=C(O)c1cnc(N2CCC(c3cc(Cl)c(Cl)c(Cl)c3)(C(F)(F)F)C2)nc1C(F)(F)F
2-[3-(3,4,5-trichlorophenyl)-3-(trifluoromethyl)-pyrrolidin-1-yl]-4-(trifluoromethyl)pyrimidine-5-carboxylic acid
收率 92.3%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度After cooling
  2. 2
    萃取extracted with ethyl acetate
  3. 3
    干燥The organic layer was dried over magnesium sulfate
  4. 4
    其他The solvent was evaporated off under reduced pressure

实验过程

Ethyl 2-[3-(3,4,5-trichlorophenyl)-3-(trifluoromethyl)pyrrolidin-1-yl]-4-(trifluoromethyl)pyrimidine-5-carboxylate (2.4 g) was added to a mixture solution comprising 1,4-dioxane (40 mL) and an aqueous solution (40 mL) of sodium hydroxide (2.0 g), and then heated at 80° C. for 10 hours. After cooling, the reaction solution was poured over ice water, acidified by adding concentrated hydrochloric acid, and then extracted with ethyl acetate. The organic layer was dried over magnesium sulfate. The solvent was evaporated off under reduced pressure to obtain the title compound (2.1 g, 92%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09271499B2uspto-grants-2016_03