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Sodium hydride → Dimethyl 4-(5-chloro-3-methylbenzo[b]thiophene-2-sulfonylamino)isophthalate

HRID 1790221
ノート
印刷プレビュー

反応式

HRID 1790221 の反応式
[NH2:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][C:3]=1[C:12]([O:14][CH3:15])=[O:13].[H-].[Na+].[Cl:18][C:19]1[CH:32]=[CH:31][C:22]2[S:23][C:24]([S:27](Cl)(=[O:29])=[O:28])=[C:25]([CH3:26])[C:21]=2[CH:20]=1>C1COCC1>[Cl:18][C:19]1[CH:32]=[CH:31][C:22]2[S:23][C:24]([S:27]([NH:1][C:2]3[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][C:3]=3[C:12]([O:14][CH3:15])=[O:13])(=[O:28])=[O:29])=[C:25]([CH3:26])[C:21]=2[CH:20]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 24758Sodium hydride2 回HCID 27357565-Chloro-3-methylbenzo(b)thiophene-2-sulfonyl chlorideHCID 11095854Dimethyl 4-aminoisophthalate

生成物 1

HCID 22041453Dimethyl 4-(5-chloro-3-methylbenzo[b]thiophene-2-sulfonylamino)isophthalate収率 29.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Into 8 mL of THF was dissolved 115 mg of dimethyl 4-aminoisophthalate, followed by addition of 22 mg of sodium hydride (oily, 60%). After 20 minutes of stirring at room temperature, 130 mg of 5-chloro-2-chlorosulfonyl-3-methylbenzo[b]thiophene was added at the same temperature, followed by 30 minutes of stirring at room temperature. Further, 26 mg of sodium hydride (oily, 60%) was added and the whole was heated under refluxing for 6 hours. After confirmation of disappearance of the starting material, the reaction was terminated by adding saturated aqueous ammonium chloride solution at 0° C., followed by extraction with ethyl acetate. The organic layer was washed with saturated brine and then dried over anhydrous sodium sulfate. The solvent was removed by evaporation and the residue was purified by silica gel column chromatography (ethyl acetate/hexane 1/1) to obtain 62 mg of the title compound as light yellow amorphous.

後処理

  1. waitfollowed by 30 minutes
  2. stirringof stirring at room temperature
  3. temperaturethe whole was heated
  4. temperatureunder refluxing for 6 hours
  5. customAfter confirmation of disappearance of the starting material, the reaction was terminated
  6. additionby adding saturated aqueous ammonium chloride solution at 0° C.
  7. extractionfollowed by extraction with ethyl acetate
  8. washThe organic layer was washed with saturated brine
  9. dry with materialdried over anhydrous sodium sulfate
  10. customThe solvent was removed by evaporation
  11. customthe residue was purified by silica gel column chromatography (ethyl acetate/hexane 1/1)

出典と根拠

ORDレコード
ord-46eef5de2b1e4935b5dd697656646385
出典データセット
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07071220B2

反応ノート

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