5-((Dimethylamino)methyl)-2-furanmethanol → 2-[[5-(Dimethylamino)methyl-2-furanyl]methoxy]ethanamine

HRID 65744

反応式

HRID 65744 の反応式
Cl.Cl[CH2:3][CH2:4][NH2:5].CC(C)([O-])C.[K+].[CH3:12][N:13]([CH2:15][C:16]1[O:20][C:19]([CH2:21][OH:22])=[CH:18][CH:17]=1)[CH3:14]>CN(C)C=O>[CH3:14][N:13]([CH2:15][C:16]1[O:20][C:19]([CH2:21][O:22][CH2:3][CH2:4][NH2:5])=[CH:18][CH:17]=1)[CH3:12]

参加物

5

反応物 3

HCID 849065-((Dimethylamino)methyl)-2-furanmethanolHCID 97937372-Chloroethylamine hydrochlorideHCID 23665647Potassium tert-butoxide

生成物 1

HCID 202133122-[[5-(Dimethylamino)methyl-2-furanyl]methoxy]ethanamine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 2-chloroethylamine hydrochloride (6.25 g) in dry dimethylformamide was added dropwise to a stirred, cooled solution of potassium tert-butoxide (8.96 g) and 5-(dimethylamino)methyl-2-furanmethanol (12.4 g) in the same solvent. After 2 hr solvent was removed, the residue basified and extracted with ethyl acetate. The residue after removal of solvent was treated in ethanol with ethanolic oxalic acid. The crystalline salt was recrystallised from ethanol to give 2-[[5-(dimethylamino)methyl-2-furanyl]methoxy]ethanamine, bis oxalate, m.p. 130°-133° (3.05 g).

後処理

  1. customAfter 2 hr solvent was removed
  2. extractionthe residue basified and extracted with ethyl acetate
  3. customThe residue after removal of solvent
  4. additionwas treated in ethanol with ethanolic oxalic acid
  5. customThe crystalline salt was recrystallised from ethanol

出典と根拠

ORDレコード
ord-31301e6e1b0b47f1a66e9b48bc759747
出典データセット
uspto-grants-1978_12
特許番号
US04128658

関連ノート

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