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Methyl 2-nitroacetate → (E)-Methyl-2-nitro-3-(2,4,6-trimethoxyphenyl)acrylate

HRID 553269
ノート
印刷プレビュー

反応式

HRID 553269 の反応式
[CH3:1][O:2][C:3]1[CH:10]=[C:9]([O:11][CH3:12])[CH:8]=[C:7]([O:13][CH3:14])[C:4]=1[CH:5]=O.S([O-])([O-])(=O)=O.[Mg+2].C([O-])(=O)C.[NH4+].[N+:26]([CH2:29][C:30]([O:32][CH3:33])=[O:31])([O-:28])=[O:27]>ClCCl.O>[CH3:33][O:32][C:30](=[O:31])/[C:29](/[N+:26]([O-:28])=[O:27])=[CH:5]\[C:4]1[C:3]([O:2][CH3:1])=[CH:10][C:9]([O:11][CH3:12])=[CH:8][C:7]=1[O:13][CH3:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 17206Methyl 2-nitroacetateHCID 24083Sulfuric acid magnesium salt (1:1)HCID 700192,4,6-TrimethoxybenzaldehydeHCID 517165Ammonium Acetate

生成物 1

HCID 86641484(E)-Methyl-2-nitro-3-(2,4,6-trimethoxyphenyl)acrylate

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6344Dichloromethane溶媒

実験手順

2,4,6-trimethoxybenzaldehyde (20.75 g, 0.105 mol) was dissolved in dichloromethane (300 mL) and to this solution magnesium sulphate (15 g, 0.124 mol), ammonium acetate (10 g, 0.129 mol) and methyl nitroacetate (12.60 g, 0.105 mol) were added and stirred at room temperature for 2 hours. At the end of two hours, water (300 mL) was added to the reaction mass, the organic layer was separated and the aqueous layer extracted with dichloromethane (2×100 mL). The organic layers were combined and concentrated under reduced pressure to give a solid, which was crystallized from methanol (100 mL).

後処理

  1. additionwere added
  2. customthe organic layer was separated
  3. extractionthe aqueous layer extracted with dichloromethane (2×100 mL)
  4. concentrationconcentrated under reduced pressure
  5. customto give a solid, which
  6. customwas crystallized from methanol (100 mL)

出典と根拠

ORDレコード
ord-12de784fbfca4daea0727a347296f570
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07951961B2

反応ノート

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