Reaktion #630755

Reaktionsgleichung

1-methylcyclopropanecarbonyl chloride

3-chloro-4-trifluoromethoxyaniline

triethylamine

→

N-(3-chloro-4-trifluoromethoxyphenyl)-1-methylcyclopropanecarboxamide

Ausbeute 89.2%

Lösungsmittel

methylene chloride

methylene chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturice-cooling
2. 2
   workup.STIRRINGAfter stirring at room temperature for 1 hour
3. 3
   Waschenthe reaction mixture was washed with 1 N hydrochloric acid, sodium hydrogen carbonate solution and saturated sodium chloride solution
4. 4
   Trocknendried over anhydrous magnesium sulfate
5. 5
   Einengenconcentrated
6. 6
   SonstigeThe crude crystals (2.9 g) were recrystallized from ethanol

Vorschrift

To a solution of 3-chloro-4-trifluoromethoxyaniline (2.1 g) in methylene chloride (50 ml), triethylamine (1.1 g) was added, and a solution of 1-methylcyclopropanecarbonyl chloride (1.2 g) in methylene chloride was dropwise added thereto while stirring and ice-cooling. After stirring at room temperature for 1 hour, the reaction mixture was washed with 1 N hydrochloric acid, sodium hydrogen carbonate solution and saturated sodium chloride solution, dried over anhydrous magnesium sulfate and concentrated. The crude crystals (2.9 g) were recrystallized from ethanol to give N-(3-chloro-4-trifluoromethoxyphenyl)-1-methylcyclopropanecarboxamide (2.6 g). M.P., 101°-102° C.

Quelle