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Methyl 2-(4-hydroxy-3-nitrophenyl)acetate → Methyl 3-nitro-4-methallyloxyphenylacetate

HRID 328166
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HRID 328166 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([CH2:11][C:12]([O:14][CH3:15])=[O:13])[CH:7]=[CH:8][C:9]=1[OH:10])([O-:3])=[O:2].[C:16]1([CH3:30])[CH:21]=CC(S(OCC(=C)C)(=O)=O)=C[CH:17]=1.C[O-].[Na+]>CO>[N+:1]([C:4]1[CH:5]=[C:6]([CH2:11][C:12]([O:14][CH3:15])=[O:13])[CH:7]=[CH:8][C:9]=1[O:10][CH2:21][C:16](=[CH2:17])[CH3:30])([O-:3])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1473109Methyl 2-(4-hydroxy-3-nitrophenyl)acetateHCID 10942334Sodium MethoxideHCID 10955266Methallyl p-toluenesulfonate

생성물 1

HCID 21444153Methyl 3-nitro-4-methallyloxyphenylacetate

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 2.11g of methyl 3-nitro-4-hydroxyphenylacetate, 2.27g of methallyl p-toluenesulfonate was refluxed for one hour in 60ml of methanol containing natrium methoxide (natrium 0.25g). The reaction mixture was concentrated under reduced pressure and ethyl acetate and water were added to the residue. The ethyl acetate layer was isolated, and washed with water. After the extract was dried over magnesium sulfate, the solvent was distilled off and the residue was recrystallied from methanol to give the object compound having m.p. 30°- 31.5° C in a yield of 1.98g (74%).

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure and ethyl acetate and water
  2. additionwere added to the residue
  3. customThe ethyl acetate layer was isolated
  4. washwashed with water
  5. dry with materialAfter the extract was dried over magnesium sulfate
  6. distillationthe solvent was distilled off
  7. customto give the object compound

출처 및 근거

ORD 기록
ord-f9aa89924d974250968d5ec5c1499168
출처 데이터셋
uspto-grants-1977_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04016193

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