反応 #67042

ord-edede3df92e04fa488b7f19f041fa29e

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他To the reaction liquid
  2. 2
    洗浄washed with saturated brine (10 mL)
  3. 3
    乾燥dried over anhydrous magnesium sulfate
  4. 4
    その他the solvent was evaporated under reduced pressure
  5. 5
    その他The residue was purified by silica gel column chromatography (eluent: hexane-ethyl acetate)

実験手順

A mixture of methyl 2-chloro-4-(trifluoromethyl)pyrimidine-5-carboxylate (0.30 g), 2,4-dichlorobenzyl amine (818 μL), and 1,4-dioxane (3 mL) was stirred at room temperature for 21 hours. To the reaction liquid was added ethyl acetate (30 mL), washed with saturated brine (10 mL), and dried over anhydrous magnesium sulfate, and then the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: hexane-ethyl acetate) to obtain methyl 2-(2,4-dichlorobenzylamino)-4-(trifluoromethyl)pyrimidine-5-carboxylate (446 mg) as a colorless solid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08524727B2uspto-grants-2013_09