Water → 2-Chloro-4-(3-trifluoromethylpyrazolyl) benzonitrile

HRID 25311

반응식

HRID 25311 반응식
[F:1][C:2]([F:9])([F:8])[C:3]1[CH:7]=[CH:6][NH:5][N:4]=1.[Cl:10][C:11]1[CH:18]=[C:17](F)[CH:16]=[CH:15][C:12]=1[C:13]#[N:14].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[Cl:10][C:11]1[CH:18]=[C:17]([C:7]2[C:3]([C:2]([F:9])([F:8])[F:1])=[N:4][NH:5][CH:6]=2)[CH:16]=[CH:15][C:12]=1[C:13]#[N:14]

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 1090002-Chloro-4-fluorobenzonitrileHCID 18070343-(Trifluoromethyl)pyrazole

생성물 1

HCID 1785096022-Chloro-4-(3-trifluoromethylpyrazolyl) benzonitrile수율 92%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

2.5 g (18.4 mmol) of 3-trifluoromethylpyrazole, 2.9 g (18.4 mmol) of 2-chloro-4-fluorobenzonitrile and 2.8 g (20.2 mmol) of potassium carbonate in 20 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. After washed with n-hexane, the residue afforded 4.6 g of 2-chloro-4-(3-trifluoromethylpyrazolyl)benzonitrile (yield 92.0%) as a white powder, which was used in Reference Example 3 as the starting material.

후처리

  1. extractionthe organic matters were extracted with 50 ml of ethyl acetate twice
  2. washwashed with 50 ml of water twice
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationthe ethyl acetate was distilled off under reduced pressure
  5. washAfter washed with n-hexane

출처 및 근거

ORD 기록
ord-2fe98f7283704ed6a21b2243dd513d90
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06858639B2

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