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

HRID 328166
ノート
印刷プレビュー

反応式

HRID 328166 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 21444153Methyl 3-nitro-4-methallyloxyphenylacetate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-f9aa89924d974250968d5ec5c1499168
出典データセット
uspto-grants-1977_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04016193

反応ノート

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