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Ethylamine → HCID 19353515, 화합물

HRID 1584218
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HRID 1584218 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][C:12]2[CH:17]=[C:16]([NH:18][CH3:19])[N:15]=[C:14](Br)[CH:13]=2)(=[O:10])=[O:9])=[CH:4][CH:3]=1.[CH2:21]([NH2:23])[CH3:22]>>[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][C:12]2[CH:17]=[C:16]([NH:18][CH3:19])[N:15]=[C:14]([NH:23][CH2:21][CH3:22])[CH:13]=2)(=[O:10])=[O:9])=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 6341Ethylamine2회HCID 10689660HCID 10689660, 화합물

생성물 1

HCID 19353515HCID 19353515, 화합물수율 2.5%

실험 절차

2.5 g (0.007 mol) of 4-amino-N-(2-bromo-6-methylamino-pyridin-4-yl)-benzenesulfonamide were stirred with 80 ml of ethylamine in an autoclave at 160° C. for 40 hours. The residual ethylamine was left to evaporate and the residue was chromatographed on silica gel with ethyl acetate/hexane 1:2, then 2:3 and finally 1:1. The thus-obtained 0.67 g of brown oil was suspended in 200 ml of 1N NaOH, suction filtered and the filtrate was neutralized with 1N HCl. It was again suction filtered, the filtrate was saturated with NaCl and extracted with ethyl acetate. The organic phase was dried. There was obtained 0.055 g (2.5%) of 4-amino-N-(2-ethylamino-6-methylamino-pyridin-4-yl)-benzenesulfonamide as pale brown crystals; MS (ISN): me/e=320 (C14H18N5O2S-).

후처리

  1. customto evaporate
  2. custom
the residue was chromatographed on silica gel with ethyl acetate/hexane 1:2
  • filtrationsuction filtered
  • filtrationfiltered
  • extractionextracted with ethyl acetate
  • customThe organic phase was dried
  • 출처 및 근거

    ORD 기록
    ord-014bfd2d448e45d3babe39710171320d
    출처 데이터셋
    uspto-grants-1999_08
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US05932599

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