Water → HCID 178509603, 화합물

HRID 25303

반응식

HRID 25303 반응식
Cl[C:2]1[CH:9]=[C:8]([C:10]2[C:11]([C:15]([F:18])([F:17])[F:16])=[N:12][NH:13][CH:14]=2)[CH:7]=[CH:6][C:3]=1[C:4]#[N:5].[S-2:19].[Na+].[Na+].O>CN(C)C=O>[SH:19][C:2]1[CH:9]=[C:8]([C:10]2[C:11]([C:15]([F:18])([F:17])[F:16])=[N:12][NH:13][CH:14]=2)[CH:7]=[CH:6][C:3]=1[C:4]#[N:5]

참가 물질

5

반응물 3

HCID 962WaterHCID 14804Sodium SulfideHCID 1785096022-Chloro-4-(3-trifluoromethylpyrazolyl) benzonitrile

생성물 1

HCID 178509603HCID 178509603, 화합물수율 97.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

5.0 g (18.4 mmol) of 2-chloro-4-(3-trifluoromethylpyrazolyl)benzonitrile in N,N-dimethylformamide was stirred together with 1.86 g (23.9 mmol) of sodium sulfide at 120° C. for 30 minutes. The reaction mixture was cooled to room temperature, mixed with 100 ml of water, washed with 30 ml of ethyl acetate, and the aqueous layer was adjusted at pH 5-6 with citric acid, and 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. The ethyl acetate was distilled off under reduced pressure to obtain 2-mercapto-4-(3-trifluoromethylpyrazolyl)benzonitrile (yield 97.6%) as a pale yellow powder, which was used in Example 1 (2) as the starting material.

후처리

  1. washwashed with 30 ml of ethyl acetate
  2. extractionextracted with 50 ml of ethyl acetate twice
  3. washwashed with 50 ml of water twice
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationThe ethyl acetate was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-65d3528a2c174145a0986568ff963a1a
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06858639B2

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