反応 #67044

反応方程式

methyl 2-(2,4-dichlorobenzylamino)-4-(trifluoromethyl)pyrimidine-5-carboxylate

potassium hydroxide

→

2-(2,4-dichlorobenzylamino)-4-(trifluoromethyl)pyrimidine-5-carboxylic acid

収率 96.3%

溶媒

ethanol

ethanol

反応条件

後処理

1. 1
   温度under heating
2. 2
   温度with reflux for 5 hours
3. 3
   その他The reaction liquid
4. 4
   濃縮was concentrated under reduced pressure, water (70 mL)
5. 5
   workup.ADDITIONwas added to the residue
6. 6
   抽出The product was extracted with ethyl acetate (200 mL) twice
7. 7
   乾燥the organic layer was dried over anhydrous magnesium sulfate
8. 8
   その他The solvent was evaporated under reduced pressure

実験手順

To a mixture of methyl 2-(2,4-dichlorobenzylamino)-4-(trifluoromethyl)pyrimidine-5-carboxylate (443 mg) and ethanol (7 mL) was added a solution of potassium hydroxide (200 mg) in ethanol (4 mL), and the mixture was stirred under heating with reflux for 5 hours. The reaction liquid was concentrated under reduced pressure, water (70 mL) was added to the residue, and the liquid property was made acidic (pH 1) with concentrated hydrochloric acid. The product was extracted with ethyl acetate (200 mL) twice, and then the organic layer was dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure to obtain 2-(2,4-dichlorobenzylamino)-4-(trifluoromethyl)pyrimidine-5-carboxylic acid (411 mg) as a colorless powder.

出典