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Diethyl Ether → HCID 18670585、化合物

HRID 1059286
ノート
印刷プレビュー

反応式

HRID 1059286 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

HCID 18670585HCID 18670585、化合物収率 104.7%

試薬・触媒・溶媒 2

HCID 74505Methyltriphenyliphosphonium bromide触媒HCID 1140Toluene
溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-c380773cb2894b709aa8aeababa6fd25
出典データセット
uspto-grants-2003_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06518423B1

反応ノート

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