Phosphorus sulfide (P2S5) → HCID 22041438, 화합물

HRID 1790231노트

반응식

HRID 1790231 반응식
[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

참가 물질

4

반응물 2

HCID 14817Phosphorus sulfide (P2S5)HCID 22041454HCID 22041454, 화합물

생성물 1

HCID 22041438HCID 22041438, 화합물수율 77%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-9673436fbafd4e999edf685887af37da
출처 데이터셋
uspto-grants-2006_07
특허 번호
US07071220B2

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