反应详情

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.

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