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Acetic Anhydride → HCID 21409904, 화합물

HRID 1283537
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HRID 1283537 반응식
[CH3:1][NH:2][CH2:3][C:4]1([N:10]2[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]2)[CH2:9][CH2:8][CH2:7][CH2:6][CH2:5]1.[C:16](OC(=O)C)(=[O:18])[CH3:17]>>[CH3:1][N:2]([CH2:3][C:4]1([N:10]2[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]2)[CH2:9][CH2:8][CH2:7][CH2:6][CH2:5]1)[C:16](=[O:18])[CH3:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 7918Acetic AnhydrideHCID 21409890N-Methyl-1-[1-(piperidin-1-yl)cyclohexyl]methanamine

생성물 1

HCID 21409904HCID 21409904, 화합물

실험 절차

A mixture of 1-[1-[(methylamino)methyl]cyclohexyl]-piperidine (1.0 g., 0.005 mole) and acetic anhydride (10 ml) was heated on a steam-bath for 30 mins. The solution was evaporated to dryness and water (5 ml) was added to the residue. A saturated solution of sodium carbonate (10 ml) was added and the alkaline solution was extracted with chloroform (50 ml × 3) and dried (anhyd. Na2SO4). The chloroform solution was evaporated to dryness and the oily residue re-evaporated with ether. This was dissolved in petroleum ether (60°-80°C), treated with decol. charcoal, and filtered (hyflo). The combined filtrates were evaporated to dryness to give N-methyl-N-[(piperidino cyclohexyl)methyl]acetamide (1.3 g.).

후처리

  1. temperaturewas heated on a steam-bath for 30 mins
  2. customThe solution was evaporated to dryness and water (5 ml)
  • additionwas added to the residue
  • additionA saturated solution of sodium carbonate (10 ml) was added
  • extractionthe alkaline solution was extracted with chloroform (50 ml × 3)
  • dry with materialdried (anhyd. Na2SO4)
  • customThe chloroform solution was evaporated to dryness
  • customthe oily residue re-evaporated with ether
  • dissolutionThis was dissolved in petroleum ether (60°-80°C)
  • additiontreated with decol
  • filtrationcharcoal, and filtered (hyflo)
  • customThe combined filtrates were evaporated to dryness
  • 출처 및 근거

    ORD 기록
    ord-d3caae3fcb4647b69a3703f4c941c91c
    출처 데이터셋
    uspto-grants-1976_08
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US03975443

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