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2,3-Dichlorobenzaldehyde → HCID 54186754、化合物

HRID 620952
ノート
印刷プレビュー

反応式

HRID 620952 の反応式
C[O-].[Na+].[Cl-].[CH3:5][O:6][CH2:7][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.[Cl:27][C:28]1[C:35]([Cl:36])=[CH:34][CH:33]=[CH:32][C:29]=1[CH:30]=O>C(O)C>[CH3:5][O:6][CH:7]=[CH:30][C:29]1[CH:32]=[CH:33][CH:34]=[C:35]([Cl:36])[C:28]=1[Cl:27]
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 357452,3-DichlorobenzaldehydeHCID 2723798Methoxymethyl-triphenylphosphonium chlorideHCID 10942334Sodium Methoxide

生成物 1

HCID 54186754HCID 54186754、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

47.3 g of sodium methylate are introduced into 1.5 liters of absolute ethanol. There are then added portionwise, at room temperature, firstly 300.0 g of methoxymethyltriphenylphosphonium chloride and afterwards 142.5 g of 2,3-dichlorobenzaldehyde, and the reaction mixture is heated at 70° C. for about 60 hours. After cooling to room temperature, the mixture is filtered, and the filtrate is concentrated in vacuo. The residue is taken up in pentane, washed, again concentrated by evaporation, and filtered over SiO2 with dichloromethane. Excess solvent is removed in vacuo. There is thus obtained β-methoxy-2,3-dichlorostyrene as a 1:1 (E/Z) mixture in the form of a light-yellow oil.

後処理

  1. additionThere are then added portionwise, at room temperature
  2. filtrationthe mixture is filtered
  3. concentrationthe filtrate is concentrated in vacuo
  4. washwashed
  5. concentrationagain concentrated by evaporation
  6. filtrationfiltered over SiO2 with dichloromethane
  7. customExcess solvent is removed in vacuo

出典と根拠

ORDレコード
ord-8224d9011c62414fa19ee00f6a8630e4
出典データセット
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04822919

反応ノート

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