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Diethyl Ether → HCID 18670585, 화합물

HRID 1059286
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HRID 1059286 반응식
[CH3:1]C(C)([O-])C.[K+].[CH3:7][N:8]1[CH2:15][CH:14]2[C:16](=O)[CH:10]([CH2:11][CH2:12][CH2:13]2)[CH2:9]1.CCOCC>[Br-].C[P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.C1(C)C=CC=CC=1>[CH3:7][N:8]1[CH2:15][CH:14]2[C:16](=[CH2:1])[CH:10]([CH2:11][CH2:12][CH2:13]2)[CH2:9]1
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참가 물질

6

반응물 3

HCID 3283Diethyl EtherHCID 5414983-Methyl-3-azabicyclo[3.3.1]nonan-9-oneHCID 23665647Potassium tert-butoxide

생성물 1

HCID 18670585HCID 18670585, 화합물수율 104.7%

시약·촉매·용매 2

HCID 74505Methyltriphenyliphosphonium bromide촉매HCID 1140Toluene
용매

실험 절차

To a solution of 6.9 g of methyltriphenyl phosphonium bromide in toluene (30 ml) was added 2.2 g of potassium tert-butoxide at 0° C. and the resulting mixture was stirred for 30 minutes. Next, 3.0 g of 3-methyl-3-azabicyclo[3.3.1]nonan-9-one was added thereto and the mixture was reacted for 1 hour. After adding ether, the reaction mixture was washed with a saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate. After filtering and concentrating, the residue was purified by silica gel column chromatography (eluted with ether/n-hexane) to thereby give 3.1 g of the title compound as a yellow oily substance.

후처리

  1. customthe mixture was reacted for 1 hour
  2. washthe reaction mixture was washed with a saturated aqueous solution of sodium chloride
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationAfter filtering
  5. concentrationconcentrating
  6. customthe residue was purified by silica gel column chromatography (eluted with ether/n-hexane)

출처 및 근거

ORD 기록
ord-c380773cb2894b709aa8aeababa6fd25
출처 데이터셋
uspto-grants-2003_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06518423B1

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