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Nitroethane → 1-Methylsulfanyl-4-(2-nitro-propenyl)-benzene

HRID 462697
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HRID 462697 반응식
[CH3:1][S:2][C:3]1[CH:10]=[CH:9][C:6]([CH:7]=O)=[CH:5][CH:4]=1.[N+:11]([CH2:14][CH3:15])([O-:13])=[O:12].C(N)CCC>C(O)C>[CH3:1][S:2][C:3]1[CH:10]=[CH:9][C:6]([CH:7]=[C:14]([N+:11]([O-:13])=[O:12])[CH3:15])=[CH:5][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6587NitroethaneHCID 8007ButylamineHCID 769854-(Methylthio)benzaldehyde

생성물 1

HCID 28259171-Methylsulfanyl-4-(2-nitro-propenyl)-benzene수율 44.5%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

The intermediate 1-[4-(methylthio)phenyl]-2-nitro-1-propene was prepared as follows: [U.S. Pat. No. 3,117,160, Example V]; a mixture containing 15.2 g of 4-(methylthio)benzaldehyde, 7.5 g of nitroethane, 0.73 g of n-butylamine and 40 ml of absolute ethanol was refluxed with stirring for 21 hours and the solvent then removed by distilling in vacuo. The residue was recrystallized from absolute ethanol (total volume of 60 ml) washed with a small quantity of cold ethanol and dried in vacuo at room temperature to produce 9.3 g of 1-[4-(methylthio)phenyl]-2-nitro-1-propene, m.p. 74°-76° C.

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후처리

  1. customThe intermediate 1-[4-(methylthio)phenyl]-2-nitro-1-propene was prepared
  2. temperaturewas refluxed
  3. customthe solvent then removed
  4. distillationby distilling in vacuo
  5. customThe residue was recrystallized from absolute ethanol (total volume of 60 ml)
  6. washwashed with a small quantity of cold ethanol
  7. customdried in vacuo at room temperature

출처 및 근거

ORD 기록
ord-e7dc28bb41c44a029e109f4229f2e877
출처 데이터셋
uspto-grants-1985_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04517192

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