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Potassium Carbonate → 4-[[2-(Diethylamino)ethyl]thio]benzenamine

HRID 1164954
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HRID 1164954 반응식
[CH2:1]([N:3]([CH2:16][CH3:17])[CH2:4][CH2:5][S:6][C:7]1[CH:12]=[CH:11][C:10]([N+:13]([O-])=O)=[CH:9][CH:8]=1)[CH3:2].O.O.[Sn](Cl)Cl.C(=O)([O-])[O-].[K+].[K+]>C(O)C.O>[CH2:16]([N:3]([CH2:1][CH3:2])[CH2:4][CH2:5][S:6][C:7]1[CH:8]=[CH:9][C:10]([NH2:13])=[CH:11][CH:12]=1)[CH3:17]
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참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 61436Stannous chloride dihydrateHCID 19863411N,N-diethyl-2-[(4-nitrophenyl)thio]ethanamine

생성물 1

HCID 198633934-[[2-(Diethylamino)ethyl]thio]benzenamine

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

To a solution of 7.4 g (29 mmol) of N,N-diethyl-2-[(4-nitrophenyl)thio]ethanamine in 150 mL of ethanol add 32.8 g (140 mmol) of tin(II) chloride dihydrate. Reflux the reaction mixture for about 5 h. After this time, cool the reaction mixture to room temperature and carefully add the mixture to a solution of 75 g (0.54 mol) of potassium carbonate in 500 mL of water. Extract the mixture with 3×500 mL of ethyl acetate. Combine the organic extracts and wash with 2×350 mL of saturated aqueous sodium chloride solution. Dry the organic extracts over anhydrous sodium sulfate. Remov the drying agent by filtration and evaporate the solvent in vacuo to obtain the title compound.

후처리

  1. temperatureReflux the reaction mixture for about 5 h
  2. extractionExtract the mixture with 3×500 mL of ethyl acetate
  3. washwash with 2×350 mL of saturated aqueous sodium chloride solution
  4. dry with materialDry the organic extracts over anhydrous sodium sulfate
  5. customRemov the drying agent
  6. filtrationby filtration
  7. customevaporate the solvent in vacuo

출처 및 근거

ORD 기록
ord-dcd8c592af6e47fb9304c6928fae98a8
출처 데이터셋
uspto-grants-1990_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04906634

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