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Dimethyl Sulfoxide → HCID 67401611、化合物

HRID 1186302
ノート
印刷プレビュー

反応式

HRID 1186302 の反応式
Cl[C:2]1[C:11]([O:12][CH:13]([C:18]2[CH:19]=[N:20][CH:21]=[CH:22][CH:23]=2)[C:14]([F:17])([F:16])[F:15])=[N:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.CS(C)=O.[C:28]([C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=1[S:36]([NH2:39])(=[O:38])=[O:37])#[N:29].C(=O)([O-])[O-].[K+].[K+]>C(O)(=O)C>[C:28]([C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=1[S:36]([NH:39][C:2]1[C:11]([O:12][CH:13]([C:18]2[CH:19]=[N:20][CH:21]=[CH:22][CH:23]=2)[C:14]([F:17])([F:16])[F:15])=[N:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1)(=[O:38])=[O:37])#[N:29]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 679Dimethyl SulfoxideHCID 11430Potassium CarbonateHCID 15110752-CyanobenzenesulfonamideHCID 86657923HCID 86657923、化合物

生成物 1

HCID 67401611HCID 67401611、化合物収率 70%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

According to Example 132, by use of 2-chloro-3-[2,2,2-trifluoro-1-(pyridin-3-yl)ethoxy]-quinoxaline (Compound BJ) (70 mg, 0.21 mmol), dimethyl sulfoxide (2 mL), 2-cyanobenzenesulfonamide (38 mg, 0.21 mmol) and potassium carbonate (28 mg, 0.21 mmol), the mixture was stirred and reacted at 150° C. for 1.5 hours. The reaction mixture was allowed to cool down to room temperature, a 1% aqueous acetic acid solution was added thereto, and extraction with ethyl acetate was performed. The organic layer was washed with a saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate, and then the solvent was evaporated off under reduced pressure. The residue was subjected to slurry purification using methanol, to give 2-cyano-N-{3-[2,2,2-trifluoro-1-(pyridin-3-yl)ethoxy]-quinoxalin-2-yl}benzenesulfonamide (Compound 145) (70 mg, 70%).

後処理

  1. customreacted at 150° C. for 1.5 hours
  2. extractionextraction with ethyl acetate
  3. washThe organic layer was washed with a saturated aqueous sodium chloride solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customthe solvent was evaporated off under reduced pressure
  6. custompurification

出典と根拠

ORDレコード
ord-b5bce99ff4704c6280af6267727c4d86
出典データセット
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08673908B2

反応ノート

読み込み中…

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