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2-[2-(5-Chloro-2-methoxybenzoylamino)ethyl]-5-sulfamoylthiophene → 2-[2-(5-Chloro-2-methoxybenzoylamino)ethyl]-5-(amino-carbonylaminosulfonyl)thiophene

HRID 482023
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인쇄 미리보기

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HRID 482023 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:22][CH3:23])=[C:6]([CH:21]=1)[C:7]([NH:9][CH2:10][CH2:11][C:12]1[S:13][C:14]([S:17](=[O:20])(=[O:19])[NH2:18])=[CH:15][CH:16]=1)=[O:8].[O:24]([C:26]#[N:27])[K]>C(N(CC)CC)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:22][CH3:23])=[C:6]([CH:21]=1)[C:7]([NH:9][CH2:10][CH2:11][C:12]1[S:13][C:14]([S:17]([NH:18][C:26]([NH2:27])=[O:24])(=[O:19])=[O:20])=[CH:15][CH:16]=1)=[O:8]
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참가 물질

4

반응물 2

HCID 152886722-[2-(5-Chloro-2-methoxybenzoylamino)ethyl]-5-sulfamoylthiopheneHCID 178418250HCID 178418250, 화합물

생성물 1

HCID 152886732-[2-(5-Chloro-2-methoxybenzoylamino)ethyl]-5-(amino-carbonylaminosulfonyl)thiophene

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

299 mg (0.8 mmol of 2-[2-(5-chloro-2-methoxybenzoylamino)ethyl]-5-sulfamoylthiophene were treated with 448 mg of KOCN and 0.6 ml of triethylamine, and the mixture was then heated to reflux for 4 h. The cooled solution was filtered and evaporated to dryness. The residue was stirred with 40 ml of H2O, 25 ml of triethylamine and 25 ml of ethyl acetate. The organic phase was extracted 3 times with water/1% triethylamine. The combined aqueous phases were acidified with 2N hydrochloric acid. The precipitate formed was stirred in an ice bath for 3 hours and filtered off with suction.

후처리

  1. temperaturethe mixture was then heated
  2. temperatureto reflux for 4 h
  3. filtrationThe cooled solution was filtered
  4. customevaporated to dryness
  5. extractionThe organic phase was extracted 3 times with water/1% triethylamine
  6. customThe precipitate formed
  7. stirringwas stirred in an ice bath for 3 hours
  8. filtrationfiltered off with suction

출처 및 근거

ORD 기록
ord-27f7c6d0b37b4d85b7687858dc855a77
출처 데이터셋
uspto-grants-1998_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05792788

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