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

HRID 2372335

반응식

HRID 2372335 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 1937144-Dimethylaminomethylbenzylamine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-aab34473f26640e587e2a7aa3bf2d1dd
출처 데이터셋
uspto-grants-1992_03
특허 번호
US05098900

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