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Water → HCID 57562912, 화합물

HRID 1962242
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HRID 1962242 반응식
[NH2:1][S:2]([C:5]1[CH:6]=[C:7]([N+:14]([O-])=O)[CH:8]=[C:9]([CH3:13])[C:10]=1[O:11][CH3:12])(=[O:4])=[O:3].[NH4+].[Cl-].O>C(O)C.[Fe]>[NH2:1][S:2]([C:5]1[CH:6]=[C:7]([CH:8]=[C:9]([CH3:13])[C:10]=1[O:11][CH3:12])[NH2:14])(=[O:3])=[O:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 962WaterHCID 25517Ammonium ChlorideHCID 57562885HCID 57562885, 화합물

생성물 1

HCID 57562912HCID 57562912, 화합물

시약·촉매·용매 2

HCID 23925Iron촉매HCID 702Ethanol용매

실험 절차

The reduction of 3-aminosulfonyl-4-methoxy-5-methylnitrobenzene (0.740 g, 3 mmol) using iron powder (0.81 g, 15 mmol), NH4Cl (0.81 g, 15 mmol) in ethanol (100 mL):water (25 mL) at 60° C. for 1 hour followed by filtration through a pad of Celite gave aqueous alcoholic solution. Concentration of it followed by dilution with water afforded a solid mass, which was isolated by filtration to give 3-aminosulfonyl-4-methoxy-5-methylaniline. 1H NMR (DMSO-d6): δ 6.90 (bs, 1H), 6.55 (bs, 1H), 5.1 (bs, 2H), 3.65 (s, 3H), 2.15 (s, 3H), LCMS: purity: 94%, MS (m/e): 217 (MH+).

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후처리

  1. filtrationwater (25 mL) at 60° C. for 1 hour followed by filtration through a pad of Celite
  2. customgave aqueous alcoholic solution
  3. customafforded a solid mass
  4. customwhich was isolated by filtration

출처 및 근거

ORD 기록
ord-8ca80b90a5074b598fd16db843128503
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08415365B2

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