Phosphorus sulfide (P2S5) → HCID 22041438、化合物

HRID 1790231ノート

反応式

HRID 1790231 の反応式
[F:1][C:2]1[CH:32]=[CH:31][C:5]2[S:6][C:7]([S:10]([NH:13][C:14]3[CH:26]=[CH:25][C:17]([C:18]([NH:20][CH2:21][C:22](=O)[CH3:23])=O)=[CH:16][C:15]=3[S:27]([CH3:30])(=[O:29])=[O:28])(=[O:12])=[O:11])=[C:8]([CH3:9])[C:4]=2[CH:3]=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:34]>O1CCOCC1>[F:1][C:2]1[CH:32]=[CH:31][C:5]2[S:6][C:7]([S:10]([NH:13][C:14]3[CH:26]=[CH:25][C:17]([C:18]4[S:34][C:22]([CH3:23])=[CH:21][N:20]=4)=[CH:16][C:15]=3[S:27]([CH3:30])(=[O:29])=[O:28])(=[O:12])=[O:11])=[C:8]([CH3:9])[C:4]=2[CH:3]=1

参加物

4

反応物 2

HCID 14817Phosphorus sulfide (P2S5)HCID 22041454HCID 22041454、化合物

生成物 1

HCID 22041438HCID 22041438、化合物収率 77%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

Into 5 mL of 1,4-dioxane solution of 150 mg of 4-(5-fluoro-3-methylbenzo[b]thiophene-2-yl)sulfonamido-3-methanesulfonyl-N-(2-oxopropyl)benzamide was added 135 mg of diphosphorus pentasulfide, followed by 4.5 hours of heating under refluxing. The reaction was terminated by adding water to the reaction mixture and the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, successively and then dried over anhydrous sodium sulfate. The solvent was removed by evaporation under reduced pressure and the resulting residue was purified by silica gel column chromatography (hexane/ethyl acetate 2/1 to 1/1) to obtain 115 mg of the title compound as amorphous.

後処理

  1. temperatureof heating
  2. temperatureunder refluxing
  3. customThe reaction was terminated
  4. additionby adding water to the reaction mixture
  5. extractionthe mixture was extracted with ethyl acetate
  6. washThe organic layer was washed with water and saturated brine
  7. dry with materialsuccessively and then dried over anhydrous sodium sulfate
  8. customThe solvent was removed by evaporation under reduced pressure
  9. customthe resulting residue was purified by silica gel column chromatography (hexane/ethyl acetate 2/1 to 1/1)

出典と根拠

ORDレコード
ord-9673436fbafd4e999edf685887af37da
出典データセット
uspto-grants-2006_07
特許番号
US07071220B2

反応ノート

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