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Sodium sulfate decahydrate → 1-Methyl-1,2,3,6-tetrahydropyridine-4-carboaldehyde

HRID 1010906
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HRID 1010906 반응식
[CH3:1][N:2]1[CH2:7][CH:6]=[C:5]([C:8](OCC)=[O:9])[CH2:4][CH2:3]1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[CH3:1][N:2]1[CH2:3][CH:4]=[C:5]([CH:8]=[O:9])[CH2:6][CH2:7]1
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참가 물질

5

반응물 3

HCID 62649Sodium sulfate decahydrateHCID 566021Ethyl 1-methyl-1,2,3,6-tetrahydro-4-pyridinecarboxylateHCID 21226445Aluminium lithium hydride

생성물 1

HCID 212843781-Methyl-1,2,3,6-tetrahydropyridine-4-carboaldehyde수율 16.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution prepared by dissolving 1.7 g of ethyl 1-methyl-1,2,3,6-tetrahydro-4-pyridinecarboxylate in 20 mL of tetrahydrofuran, 773 mg of lithium aluminum hydride was added, and the mixture was stirred for 1 hour at room temperature. The reaction solution was cooled to 0° C., and then sodium sulfate decahydrate was slowly added until there are no bubbles, and stirred overnight at room temperature. The insolubles were filtered and the filtrate was concentrated under reduced pressure. The obtained residue was dissolved in 40 mL of chloroform, then 2 g of manganese dioxide was added thereto, and the mixture was stirred overnight at room temperature. The insolubles were filtered through celite, the filtrate was concentrated under reduced pressure, and the resulting residue was purified by silica gel column chromatography (eluent: chloroform/methanol=100/0-90/10), to obtain 212 mg of 1-methyl-1,2,3,6-tetrahydropyridine-4-carboaldehyde [34-1] (hereinafter, referred to as the compound [34-1]).

후처리

  1. customTo a solution prepared
  2. additionwas added
  3. temperatureThe reaction solution was cooled to 0° C.
  4. stirringstirred overnight at room temperature
  5. filtrationThe insolubles were filtered
  6. concentrationthe filtrate was concentrated under reduced pressure
  7. dissolutionThe obtained residue was dissolved in 40 mL of chloroform
  8. addition2 g of manganese dioxide was added
  9. stirringthe mixture was stirred overnight at room temperature
  10. filtrationThe insolubles were filtered through celite
  11. concentrationthe filtrate was concentrated under reduced pressure
  12. customthe resulting residue was purified by silica gel column chromatography (eluent: chloroform/methanol=100/0-90/10)

출처 및 근거

ORD 기록
ord-ba6e10397bc04c8dac1a6db9689c18cb
출처 데이터셋
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07977336B2

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