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Ammonium Chloride → N~1~-benzyl-4-nitro-1,2-benzenediamine

HRID 1709199
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HRID 1709199 반응식
[CH2:1]([NH:8][C:9]1[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[CH:11][C:10]=1[N+:18]([O-])=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl-].[NH4+].O.[S-2].[Na+].[Na+]>CO>[CH2:1]([NH:8][C:9]1[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[CH:11][C:10]=1[NH2:18])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 346028N-Benzyl-2,4-dinitroanilineHCID 19906495Sodium sulfide monohydrate

생성물 1

HCID 4381698N~1~-benzyl-4-nitro-1,2-benzenediamine수율 73.2%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
25 °C

실험 절차

A mixture of 2.0 g (7.3 mmol) N-benzyl-2,4-dinitroaniline, 1.50 g (28.0 mmol) ammonium chloride, 6.7 g (28.0 mmol) sodium sulfide hydrate and 100 ml methanol was refluxed for 3/4h. After cooling to 25° C. the mixture was filtered and evaporated. The product was stirred with water to give 1.3 g (73%) N-benzyl-2-amino-4-nitroaniline. 1H-NMR (CDCl3): 8.1-6.5 (8H, m), 4.9-4.3 (3H,m), 3.4 (2H, broad s).

후처리

  1. temperaturewas refluxed for 3/4h
  2. filtrationwas filtered
  3. customevaporated

출처 및 근거

ORD 기록
ord-76ef26f68ee240f8b10cc1e87959e3d8
출처 데이터셋
uspto-grants-1990_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04948794

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