Water → HCID 178509604, 화합물

HRID 498966

반응식

HRID 498966 반응식
[SH:1][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].O>CS(C)=O>[S:1]([C:6]1[CH:7]=[C:8]([C:10]2[C:11]([C:15]([F:16])([F:17])[F:18])=[N:12][NH:13][CH:14]=2)[CH:9]=[CH:2][C:3]=1[C:4]#[N:5])[C:2]1[CH:9]=[C:8]([C:10]2[C:11]([C:15]([F:16])([F:18])[F:17])=[N:12][NH:13][CH:14]=2)[CH:7]=[CH:6][C:3]=1[C:4]#[N:5]

참가 물질

4

반응물 2

HCID 962WaterHCID 178509603HCID 178509603, 화합물

생성물 1

HCID 178509604HCID 178509604, 화합물수율 46.4%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

3.0 g (11.1 mmol) of 2-mercapto-4-(3-trifluoromethylpyrazolyl)benzonitrile in 5 ml of dimethyl sulfoxide was stirred at 50° C. for 2 hours. The reaction mixture was cooled to room temperature and poured into 50 ml of water, and the organic matters were extracted with 20 ml of ethyl acetate twice. The ethyl acetate layers were combined, then washed with 30 ml of water twice and dried over anhydrous magnesium sulfate, and the ethyl acetate was distilled off under reduced pressure. Purification of the residue afforded 1.3 g of 1,1′-thiodi-[2-cyano-5-(3-trifluoromethylpyrazolyl)benzene] (yield 42.4%) as a yellow solid, which was used in Example 2 (3) as the starting material.

후처리

  1. extractionthe organic matters were extracted with 20 ml of ethyl acetate twice
  2. washwashed with 30 ml of water twice
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationthe ethyl acetate was distilled off under reduced pressure
  5. customPurification of the residue

출처 및 근거

ORD 기록
ord-8094bbf29fee4179a0c582e68c43aa00
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07767626B2

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