反应 #586155

ord-32f0f887b7e24da38c36b818c412853e

反应方程式

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

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    萃取the organic matters were extracted with 50 ml of ethyl acetate twice
  2. 2
    洗涤washed with 50 ml of water twice
  3. 3
    干燥dried over anhydrous magnesium sulfate
  4. 4
    workup.DISTILLATIONthe ethyl acetate was distilled off under reduced pressure

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07767626B2uspto-grants-2010_08