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Isobutyric Acid → 5-Chloro-2-(propan-2-yl)-1H-benzimidazole-6-sulfonamide

HRID 904849
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인쇄 미리보기

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HRID 904849 반응식
[NH2:1][C:2]1[CH:8]=[C:7]([Cl:9])[C:6]([S:10](=[O:13])(=[O:12])[NH2:11])=[CH:5][C:3]=1[NH2:4].[C:14](O)(=O)[CH:15]([CH3:17])[CH3:16].[OH-].[NH4+]>Cl>[Cl:9][C:7]1[C:6]([S:10](=[O:12])(=[O:13])[NH2:11])=[CH:5][C:3]2[NH:4][C:14]([CH:15]([CH3:17])[CH3:16])=[N:1][C:2]=2[CH:8]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6590Isobutyric AcidHCID 14923Ammonium HydroxideHCID 132896884,5-Diamino-2-chlorobenzene-1-sulfonamide

생성물 1

HCID 132897075-Chloro-2-(propan-2-yl)-1H-benzimidazole-6-sulfonamide

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

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온도
50 °C

실험 절차

To 50 ml of 4 N hydrochloric acid containing 11.8 g of 2-amino-4-chloro-5-sulfamylaniline was added 7.0 g of isobutyric acid and the suspension refluxed for 6 hours. The mixture was concentraded in vacuo to a solid and the solid then added with stirring to 38% ammonium hydroxide and stirred for thirty minutes at 50° C. The solid was collected by filtration, air dried, dissolved in isopropanol, and charcoal added. After boiling for five minutes, the suspension was filtered, cooled, and then filtered through Celite. Recrystallization from isopropanol provided 2.0 g of off-white crystals, mg 256°-259°.

후처리

  1. temperaturethe suspension refluxed for 6 hours
  2. additionthe solid then added
  3. filtrationThe solid was collected by filtration, air
  4. customdried
  5. dissolutiondissolved in isopropanol
  6. additioncharcoal added
  7. filtrationthe suspension was filtered
  8. temperaturecooled
  9. filtrationfiltered through Celite
  10. customRecrystallization from isopropanol

출처 및 근거

ORD 기록
ord-d26d8f48b12e476fafb41cc85c8e4328
출처 데이터셋
uspto-grants-1983_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04420487

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