Potassium Carbonate → HCID 22998631、化合物

HRID 854030ノート

反応式

HRID 854030 の反応式
Cl.[CH2:2]([N:4]([CH2:7][CH2:8][CH:9]1[CH2:18][CH2:17][C:16]2[C:11](=[CH:12][CH:13]=[C:14]([O:19]C)[CH:15]=2)[CH2:10]1)[CH2:5][CH3:6])[CH3:3].[OH-].[Na+].C(=O)([O-])[O-].[K+].[K+]>Br>[CH2:2]([N:4]([CH2:7][CH2:8][CH:9]1[CH2:18][CH2:17][C:16]2[C:11](=[CH:12][CH:13]=[C:14]([OH:19])[CH:15]=2)[CH2:10]1)[CH2:5][CH3:6])[CH3:3]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 14798Sodium HydroxideHCID 22998638HCID 22998638、化合物

生成物 1

HCID 22998631HCID 22998631、化合物収率 104.2%

試薬・触媒・溶媒 1

HCID 260Hydrogen Bromide溶媒

実験手順

(+)-2-[2-(N,N-Diethylamino)ethyl]-6-methoxytetralin hydrochloride (5.2 g) was added to 48% hydrobromic acid (10 ml) and the reaction mixture was heated under reflux for 4 hr and cooled. The reaction mixture was neutralized with 1 N aqueous sodium hydroxide followed by addition of 10% aqueous potassium carbonate and extracted with the combined solvent of ethyl acetate and THF (1:1). The organic layer was washed with saturated aqueous sodium chloride, dried, and concentrated. The residue was recrystallized from methanol-diisopropyl ether to obtain the titled compound (4.5 g).

後処理

  1. temperaturethe reaction mixture was heated
  2. temperatureunder reflux for 4 hr
  3. temperaturecooled
  4. extractionextracted with the combined solvent of ethyl acetate and THF (1:1)
  5. washThe organic layer was washed with saturated aqueous sodium chloride
  6. customdried
  7. concentrationconcentrated
  8. customThe residue was recrystallized from methanol-diisopropyl ether

出典と根拠

ORDレコード
ord-cfe81e13caaa412e8238fad1a5aaa9bb
出典データセット
uspto-grants-2007_08
特許番号
US07256204B2

反応ノート

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