Stannous Chloride → 3-amino-N,N-dimethylbenzene-1-sulfonamide

HRID 1633919

반응식

HRID 1633919 반응식
[CH3:1][N:2]([CH3:15])[S:3]([C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([N+:12]([O-])=O)[CH:7]=1)(=[O:5])=[O:4].Cl[Sn]Cl>C(O)C>[NH2:12][C:8]1[CH:7]=[C:6]([S:3]([N:2]([CH3:15])[CH3:1])(=[O:5])=[O:4])[CH:11]=[CH:10][CH:9]=1

참가 물질

4

반응물 2

HCID 24479Stannous ChlorideHCID 224495N,N-Dimethyl 3-nitrobenzenesulfonamide

생성물 1

HCID 2355203-amino-N,N-dimethylbenzene-1-sulfonamide

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of the above N,N-dimethyl-3-nitro-benzenesulfonamide (20.4 mmol, 4.7 g) in ethanol (50 mL) was added SnCl2 (105 mmol, 19.9 g) and the mixture was refluxed for 1 hour. Upon cooling, the solvent was removed in vacuo. Ethyl acetate (200 mL) and NaHCO3 (sat, 100 mL) were added to the residue followed by another 200 mL ethyl acetate and 500 mL water. The phases were separated and the organic phase was washed twice with water. The organic phase was filtered, washed with water (2×100 mL) dried over MgSO4 and evaporated to leave the title compound.

후처리

  1. temperaturethe mixture was refluxed for 1 hour
  2. temperatureUpon cooling
  3. customthe solvent was removed in vacuo
  4. additionEthyl acetate (200 mL) and NaHCO3 (sat, 100 mL) were added to the residue
  5. customThe phases were separated
  6. washthe organic phase was washed twice with water
  7. filtrationThe organic phase was filtered
  8. washwashed with water (2×100 mL)
  9. dry with materialdried over MgSO4
  10. customevaporated

출처 및 근거

ORD 기록
ord-fb1a7a7b4f2a44908246eed1685ac2a6
출처 데이터셋
uspto-grants-2003_01
특허 번호
US06503949B1

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