N,N,N',N'-Tetramethylmethanediamine → 5-((Dimethylamino)methyl)-2-furanmethanol

HRID 67879

反応式

HRID 67879 の反応式
[CH3:1][N:2]([CH2:4]N(C)C)[CH3:3].[O:8]1[CH:12]=[CH:11][CH:10]=[C:9]1[CH2:13][OH:14]>C(O)(=O)C>[CH3:1][N:2]([CH2:4][C:12]1[O:8][C:9]([CH2:13][OH:14])=[CH:10][CH:11]=1)[CH3:3]

参加物

4

反応物 2

HCID 5829N,N,N',N'-TetramethylmethanediamineHCID 7361Furfuryl Alcohol

生成物 1

HCID 849065-((Dimethylamino)methyl)-2-furanmethanol収率 94%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

A solution of bis(dimethylamino)methane (112 g, 1.1 mol) in acetic acid (200 ml) was added dropwise with cooling (10° C.) to a stirred solution of 2-furanmethanol (98 g, 1.0 mol) in acetic acid (1000 ml). The mixture was stirred at room temperature for 18 hours and acetic acid was removed at 60° C. under reduced pressure. Ice (200 g) was added to the residue which was made basic with 40% aqueous sodium hydroxide (with external cooling). The mixture was extracted with ethyl acetate and the extracts were evaporated and distilled to give 5-dimethylaminomethyl-2-furanmethanol (145 g, 94%) b.p. 92°-96° C./0.2 0.5 mmHg.

後処理

  1. customacetic acid was removed at 60° C. under reduced pressure
  2. additionIce (200 g) was added to the residue which
  3. extractionThe mixture was extracted with ethyl acetate
  4. customthe extracts were evaporated
  5. distillationdistilled

出典と根拠

ORDレコード
ord-06afed7af5584767adb5809322c8679e
出典データセット
uspto-grants-1982_08
特許番号
US04347191

関連ノート

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