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Hydrochloric Acid → 4-amino-N-(2,6-dibromo-pyridin-4-yl)-benzenesulfonamide

HRID 610830
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HRID 610830 반응식
[Br:1][C:2]1[CH:7]=[C:6]([NH:8][S:9]([C:12]2[CH:17]=[CH:16][C:15]([NH:18]C(=O)C)=[CH:14][CH:13]=2)(=[O:11])=[O:10])[CH:5]=[C:4]([Br:22])[N:3]=1.Cl>[OH-].[Na+]>[NH2:18][C:15]1[CH:16]=[CH:17][C:12]([S:9]([NH:8][C:6]2[CH:7]=[C:2]([Br:1])[N:3]=[C:4]([Br:22])[CH:5]=2)(=[O:11])=[O:10])=[CH:13][CH:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 10623382N-[4-(2,6-dibromo-pyridin-4-ylsulfamoyl)-phenyl]-acetamide

생성물 1

HCID 108113474-amino-N-(2,6-dibromo-pyridin-4-yl)-benzenesulfonamide수율 86.5%

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

실험 절차

6.2 g (0.0138 mol) of N-[4-(2,6-dibromo-pyridin-4-yl-sulfamoyl)-phenyl]-acetamide were dissolved in 138 ml of 1N NaOH and boiled at reflux for 2 hours. After cooling the mixture was adjusted to pH 6 with 2N HCl and the precipitate which separated was filtered off. The material on the suction filter was washed well with water and dried. It was subsequently chromatographed on silica gel with ethyl acetate/hexane 1:2→1:1. There were obtained 4.86 g (86%) of 4-amino-N-(2,6-dibromo-pyridin-4-yl)-benzenesulfonamide as beige crystals; m.p.: 220-222° C.

후처리

  1. temperatureat reflux for 2 hours
  2. temperatureAfter cooling the mixture
  3. customthe precipitate which separated
  4. filtrationwas filtered off
  5. filtrationThe material on the suction filter
  6. washwas washed well with water
  7. customdried
  8. customIt was subsequently chromatographed on silica gel with ethyl acetate/hexane 1:2→1:1

출처 및 근거

ORD 기록
ord-4b72e52c7cc140faa8dc7f38e0533207
출처 데이터셋
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05998665

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