4-(aminomethyl)-N,N-dimethylbenzamide → 4-Dimethylaminomethylbenzylamine

HRID 2372335ノート

反応式

HRID 2372335 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][N:8]([CH3:19])[C:9]([C:11]1[CH:18]=[CH:17][C:14]([CH2:15][NH2:16])=[CH:13][CH:12]=1)=O>O1CCCC1>[CH3:19][N:8]([CH2:9][C:11]1[CH:12]=[CH:13][C:14]([CH2:15][NH2:16])=[CH:17][CH:18]=1)[CH3:7]

参加物

4

反応物 2

HCID 162278764-(aminomethyl)-N,N-dimethylbenzamideHCID 21226445Aluminium lithium hydride

生成物 1

HCID 1937144-Dimethylaminomethylbenzylamine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

Into a suspension of 0.95 g of lithium aluminum hydride and 100 ml of tetrahydrofuran, a solution obtained by dissolving 1.77 g of 4-dimethylaminocarbonylbenzylamine prepared in Reference Example 5 in 50 ml of tetrahydrofuran, was dropwise added under stirring, and the reaction solution was refluxed for 3 hours. After cooling, the reaction solution was cooled with ice, and ice pieces were gradually added to decompose the excessive reducing agent. Tetrahydrofuran was distilled off, and the residue thereby obtained was extracted with dichloromethane. The extract was washed with water and a saturated sodium chloride aqueous solution, and dried over sodium sulfate, and then the solvent was distilled off to obtain 1.13 g of the above identified compound as a pale yellow oily substance.

後処理

  1. customa solution obtained
  2. additionwas dropwise added
  3. temperaturethe reaction solution was refluxed for 3 hours
  4. temperatureAfter cooling
  5. temperaturethe reaction solution was cooled with ice, and ice pieces
  6. additionwere gradually added
  7. distillationTetrahydrofuran was distilled off
  8. customthe residue thereby obtained
  9. extractionwas extracted with dichloromethane
  10. washThe extract was washed with water
  11. dry with materiala saturated sodium chloride aqueous solution, and dried over sodium sulfate
  12. distillationthe solvent was distilled off
  13. customto obtain 1.13 g of the

出典と根拠

ORDレコード
ord-aab34473f26640e587e2a7aa3bf2d1dd
出典データセット
uspto-grants-1992_03
特許番号
US05098900

反応ノート

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