Water → HCID 178509604、化合物

HRID 498966

反応式

HRID 498966 の反応式
[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]

参加物

4

反応物 2

HCID 962WaterHCID 178509603HCID 178509603、化合物

生成物 1

HCID 178509604HCID 178509604、化合物収率 46.4%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8094bbf29fee4179a0c582e68c43aa00
出典データセット
uspto-grants-2010_08
特許番号
US07767626B2

関連ノート

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