Sodium Dithionite → 4-(4-Nitrophenoxy)benzenamine

HRID 1294055노트

반응식

HRID 1294055 반응식
[O-]S(S([O-])=O)=O.[Na+].[Na+].C([NH:12][C:13]1[CH:29]=[CH:28][C:16]([O:17][C:18]2[CH:19]=[CH:20][C:21]([N+:25]([O-:27])=[O:26])=[C:22]([CH:24]=2)N)=[CH:15][CH:14]=1)(=O)C>CCO.O>[N+:25]([C:21]1[CH:22]=[CH:24][C:18]([O:17][C:16]2[CH:28]=[CH:29][C:13]([NH2:12])=[CH:14][CH:15]=2)=[CH:19][CH:20]=1)([O-:27])=[O:26]

참가 물질

5

반응물 2

HCID 24489Sodium DithioniteHCID 13705240N-[4-(3-Amino-4-nitrophenoxy)phenyl]acetamide2회

생성물 1

HCID 802514-(4-Nitrophenoxy)benzenamine

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

Na2S2O4 (28.2 g, 160 mmol) was added to a solution of 5-(4-Acetamidophenoxy)-2-nitroaniline (Intermediate 1) (13.7 g, 48 mmol) in EtOH (600 ml) and H2O (150 ml). The yellow mixture was refluxed with vigorous stirring until the color disappeared. After cooling, the mixture was washed with brine and the product was extracted with AcOEt. The AcOEt layer was dried over MgSO4, filtered and evaporated to give intermediate 2 as a brown film (10.2 g, 83%): MS m/e 258 (M+1).

후처리

  1. temperatureThe yellow mixture was refluxed
  2. temperatureAfter cooling
  3. washthe mixture was washed with brine
  4. extractionthe product was extracted with AcOEt
  5. dry with materialThe AcOEt layer was dried over MgSO4
  6. filtrationfiltered
  7. customevaporated

출처 및 근거

ORD 기록
ord-22e04f6d98614adc8722751ee30a6b65
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07238813B2

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