Реакция #586155

ord-32f0f887b7e24da38c36b818c412853e

Уравнение реакции

O
water
FC(F)(F)c1cc[nH]n1
3-trifluoromethylpyrazol
O=Cc1ccc(F)cc1Cl
2-chloro-4-fluorobenzaldehyde
O=C([O-])[O-].[K+].[K+]
potassium carbonate
O=Cc1ccc(-c2c[nH]nc2C(F)(F)F)cc1Cl
2-chloro-4-(3-trifluoromethylpyrazolyl)benzaldehyde

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Экстракцияthe organic matters were extracted with 50 ml of ethyl acetate twice
  2. 2
    Промывкаwashed with 50 ml of water twice
  3. 3
    Сушкаdried over anhydrous magnesium sulfate
  4. 4
    workup.DISTILLATIONthe ethyl acetate was distilled off under reduced pressure

Методика

4.08 g (30.0 mmol) of 3-trifluoromethylpyrazol, 4.75 mmol (30.0 mmol) of 2-chloro-4-fluorobenzaldehyde and 4.14 g (30.0 mmol) of potassium carbonate in 30 ml of N,N-dimethylformamide were stirred at 60° C. for 2 hours. After cooling to room temperature, the reaction mixture was poured into 100 ml of water, and the organic matters were extracted with 50 ml of ethyl acetate twice. The ethyl acetate layers were combined, washed with 50 ml of water twice and dried over anhydrous magnesium sulfate, and the ethyl acetate was distilled off under reduced pressure. The residue afforded 7.18 g of 2-chloro-4-(3-trifluoromethylpyrazolyl)benzaldehyde (yield 87.2%) as a pale yellow powder, after washed with n-hexane.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07767626B2uspto-grants-2010_08