Formaldehyde → 4-Ethoxycarbonylmethoxy-2-methylene-butanal

HRID 376159ノート

反応式

HRID 376159 の反応式
[CH2:1]([O:3][C:4]([CH2:6][O:7][CH2:8][CH2:9][CH2:10][CH:11]=[O:12])=[O:5])[CH3:2].[Cl-].[CH3:14][NH2+]C.C=O>>[CH2:1]([O:3][C:4]([CH2:6][O:7][CH2:8][CH2:9][C:10](=[CH2:14])[CH:11]=[O:12])=[O:5])[CH3:2]

参加物

4

反応物 3

HCID 712FormaldehydeHCID 12954980Dimethylazanium;chlorideHCID 189915874-Ethoxycarbonylmethoxybutanal

生成物 1

HCID 189915804-Ethoxycarbonylmethoxy-2-methylene-butanal

実験手順

11 g (63.1 mmol) of 4-ethoxycarbonylmethoxybutanal, 5.8 g (71.4 mmol) of dimethylammonium chloride and 5.5 ml (73.5 mmol) of a 37% solution of formaldehyde are stirred for 1 hour at a bath temperature of 110° C. The reaction mixture is allowed to cool and extracted three times with CH2Cl2. The combined organic phases are dried over Na2SO4 and concentrated by evaporation giving 4-ethoxycarbonylmethoxy-2-methylene-butanal as a yellowish liquid which is further reacted without purification.

後処理

  1. temperatureto cool
  2. extractionextracted three times with CH2Cl2
  3. dry with materialThe combined organic phases are dried over Na2SO4
  4. concentrationconcentrated by evaporation

出典と根拠

ORDレコード
ord-89c1888346644a5bba3c894730438b7d
出典データセット
uspto-grants-1996_01
特許番号
US05488140

反応ノート

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