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Sodium Hydroxide → (2-(5-Chloro-2-methoxybenzoylamino)ethyl]-5-(methylaminocarbonylaminosulfonyl)thiophene

HRID 482022
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HRID 482022 반응식
[OH-].[Na+].[CH3:3][NH:4][C:5](=[O:10])C(Cl)(Cl)Cl.[Cl:11][C:12]1[CH:13]=[CH:14][C:15]([O:32][CH3:33])=[C:16]([CH:31]=1)[C:17]([NH:19][CH2:20][CH2:21][C:22]1[S:23][C:24]([S:27](=[O:30])(=[O:29])[NH2:28])=[CH:25][CH:26]=1)=[O:18]>CS(C)=O>[Cl:11][C:12]1[CH:13]=[CH:14][C:15]([O:32][CH3:33])=[C:16]([CH:31]=1)[C:17]([NH:19][CH2:20][CH2:21][C:22]1[S:23][C:24]([S:27]([NH:28][C:5]([NH:4][CH3:3])=[O:10])(=[O:29])=[O:30])=[CH:25][CH:26]=1)=[O:18]
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참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 2486522,2,2-Trichloro-n-methylacetamideHCID 152886722-[2-(5-Chloro-2-methoxybenzoylamino)ethyl]-5-sulfamoylthiophene

생성물 1

HCID 9802837(2-(5-Chloro-2-methoxybenzoylamino)ethyl]-5-(methylaminocarbonylaminosulfonyl)thiophene

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

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온도
65 °C

실험 절차

120 mg of powdered NaOH and 141 mg of N-methyltrichloro-acetamide (0.8 mmol) were added to 299 mg (0.8 mmol) of 2-[2-(5-chloro-2-methoxybenzoylamino)ethyl]-5-sulfamoyl-thiophene in 9 ml of DMSO. The mixture was stir 65° C. for 1.5 hours. After cooling, it was stirred into ice water of pH 2. The precipitate was filtered off with suction and taken up in CH2Cl2, and the solution was washed with water and dried using MgSO4. After evaporating the solvent, a yellow-brown crude product remained which, after treatment with CH2Cl2 /5% methanol, crystallized at -4° C.

후처리

  1. temperatureAfter cooling
  2. filtrationThe precipitate was filtered off with suction
  3. washthe solution was washed with water
  4. customdried
  5. customAfter evaporating the solvent
  6. customafter treatment with CH2Cl2 /5% methanol, crystallized at -4° C.

출처 및 근거

ORD 기록
ord-16b3842ff8724a55bc81d390fd245322
출처 데이터셋
uspto-grants-1998_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05792788

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