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Ethanol → HCID 608034, 화합물

HRID 426707
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HRID 426707 반응식
[CH3:1][S:2][C:3]1[C:8]([N+:9]([O-])=O)=[CH:7][CH:6]=[C:5]([O:12][CH3:13])[C:4]=1OC.S(S([O-])=O)([O-])=O.[Na+].[Na+].C(O)C.[C:27](=[O:30])([O-])[O-].[K+].[K+]>O>[CH3:1][S:2][C:3]1[CH:4]=[C:5]([O:12][CH3:13])[C:6]([O:30][CH3:27])=[CH:7][C:8]=1[NH2:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 702EthanolHCID 11430Potassium CarbonateHCID 24489Sodium DithioniteHCID 20389818HCID 20389818, 화합물

생성물 1

HCID 608034HCID 608034, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A reaction mixture was prepared containing 68.7 g. of 3-methylthio-4-nitroveratrole, 261 g. sodium dithionite (Na2S2O4), 1500 ml. of ethanol and 2250 ml. of water. The reaction mixture was heated at reflux temperature for about 1 hour and then cooled. The reaction mixture was then made basic with potassium carbonate and the resulting alkaline solution concentrated in vacuo to one-half its original volume. The aqueous solution was extracted twice with 2 l. portions of ether. The ether extracts were combined, dried, and the ether removed therefrom by evaporation in vacuo. The solid residue, comprising 2-methylthio-4,5-dimethoxy aniline formed in the above reaction, was recrystallized from a benzene-hexane solvent mixture to yield 33.6 g. of crystalline material melting at 69°-72° C.

후처리

  1. customA reaction mixture was prepared
  2. additioncontaining 68.7 g
  3. temperatureThe reaction mixture was heated
  4. temperatureat reflux temperature for about 1 hour
  5. temperaturecooled
  6. concentrationthe resulting alkaline solution concentrated in vacuo to one-half its original volume
  7. extractionThe aqueous solution was extracted twice with 2 l
  8. customdried
  9. customthe ether removed
  10. customby evaporation in vacuo
  11. customformed in the above reaction
  12. customwas recrystallized from a benzene-hexane solvent mixture
  13. customto yield 33.6 g

출처 및 근거

ORD 기록
ord-7e1b81fbac03489eaba50e6bed984de6
출처 데이터셋
uspto-grants-1979_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04171361

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