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N-[3-bromo-5-(4-nitrophenylsulphanyl)-phenyl]-N-methylacetamide → [3-Bromo-5-(4-nitrophenylsulphanyl)-phenyl]-methylamine

HRID 1603625
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HRID 1603625 반응식
[Br:1][C:2]1[CH:3]=[C:4]([N:18](C)[C:19](=O)C)[CH:5]=[C:6]([S:8][C:9]2[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[CH:11][CH:10]=2)[CH:7]=1>O1CCOCC1.[OH-].[Na+]>[Br:1][C:2]1[CH:3]=[C:4]([NH:18][CH3:19])[CH:5]=[C:6]([S:8][C:9]2[CH:10]=[CH:11][C:12]([N+:15]([O-:17])=[O:16])=[CH:13][CH:14]=2)[CH:7]=1
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참가 물질

4

반응물 1

HCID 19605546N-[3-bromo-5-(4-nitrophenylsulphanyl)-phenyl]-N-methylacetamide

생성물 1

HCID 19605547[3-Bromo-5-(4-nitrophenylsulphanyl)-phenyl]-methylamine수율 106.6%

시약·촉매·용매 2

HCID 14798Sodium Hydroxide용매HCID 312751,4-Dioxane용매

실험 절차

0.79 g (0.002 mol) of N-[3-bromo-5-(4-nitrophenylsulphanyl) -phenyl]-N-methylacetamide was dissolved in a mixture of 10 ml of dioxane and 10 ml of 1N NaOH and heated at reflux for 2 hrs. Subsequently, the organic solvent was distilled off and the residue was made neutral with 1N HCl and extracted with ethyl acetate. The organic phase was washed with water and sat. sodium chloride solution, dried over MgSO4, filtered, concentrated and dried. There was obtained 0.723 g (100%) of [3-bromo-5-(4-nitrophenylsulphanyl)-phenyl]-methylamine as red crystals; m.p.: 96-98° C.

후처리

  1. temperatureheated
  2. temperatureat reflux for 2 hrs
  3. distillationSubsequently, the organic solvent was distilled off
  4. extractionextracted with ethyl acetate
  5. washThe organic phase was washed with water and sat. sodium chloride solution
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customdried

출처 및 근거

ORD 기록
ord-e0a6a9633f824d9796c9d9e18ec9292c
출처 데이터셋
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05990105

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