Reaktion #67708

Reaktionsgleichung

2-cyclopropyl-4,6-bis-trifluoromethyl-benzaldehyde

intermediate 0

2-cyclopropyl-4,6-bis-trifluoromethyl-benzaldehyde

sodium chlorite

sodium dihydrogenphosphat

→

2-Cyclopropyl-4,6-bis-trifluoromethyl-benzoic acid

Lösungsmittel

tert-butylalcohol

water

2-methyl-2-butene

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe solvents were evaporated off
2. 2
   Extraktionextracted twice with tert-butyl methyl ether
3. 3
   workup.ADDITIONThe aqueous phase was adjusted to pH 2 by addition of 25% HCl
4. 4
   Extraktionextracted twice with tert-butyl methyl ether
5. 5
   SonstigeThe combined organic phases were dried on sodium sulfate
6. 6
   Filtrationfiltered
7. 7
   Sonstigeevaporated
8. 8
   SonstigeThe crude material, off-white solid (1.01 g, 54%) was used without further purification

Vorschrift

Crude 2-cyclopropyl-4,6-bis-trifluoromethyl-benzaldehyde (intermediate 0, 1.01 g, 3.58 mmol) was dissolved in 8.5 mL tert-butylalcohol and 4.5 mL 2-methyl-2-butene. At 0° C. a solution of sodium chlorite (340 mg, 3.76 mmol) and sodium dihydrogenphosphat (451 mg, 3.76 mmol) in 3 mL water was added. The reaction mixture was stirred at room temperature overnight. The solvents were evaporated off. The residue was taken up in 1N NaOH and extracted twice with tert-butyl methyl ether. The aqueous phase was adjusted to pH 2 by addition of 25% HCl and extracted twice with tert-butyl methyl ether. The combined organic phases were dried on sodium sulfate, filtered and evaporated. The crude material, off-white solid (1.01 g, 54%) was used without further purification.

Quelle