HCID 11043960、化合物 → AH-9700 free base

HRID 1457313ノート

反応式

HRID 1457313 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[CH3:12])[CH:8](O)[CH:7]([CH2:14][CH2:15][N:16]1[CH2:20][CH2:19][CH2:18][CH2:17]1)[CH2:6][CH2:5]2>Cl.C(O)C>[CH3:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[CH3:12])[CH:8]=[C:7]([CH2:14][CH2:15][N:16]1[CH2:20][CH2:19][CH2:18][CH2:17]1)[CH2:6][CH2:5]2

参加物

4

反応物 1

HCID 11043960HCID 11043960、化合物

生成物 1

HCID 9816524AH-9700 free base収率 64.7%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 702Ethanol溶媒

実験手順

1,2,3,4-Tetrahydro-6,7-dimethyl-2-[2-(1-pyrrolidinyl)ethyl]-1-naphthalenol (24.0 g) was dissolved in a 30% solution of hydrogen chloride in ethanol (240 ml), and the mixture was refluxed for one hour. The reaction solution was concentrated under reduced pressure, and the residue was dissolved in water. The mixture was basified with potassium carbonate, and extracted with ethyl acetate. The extract was washed with water and a saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate, and concentrated under reduced pressure to remove the solvent. The residue was purified by silica gel column chromatography (eluent; chloroform:methanol=10:1), and the fractions containing the desired compound were combined, and concentrated under reduced pressure to give the desired compound (14.5 g) as an oily product.

後処理

  1. temperaturethe mixture was refluxed for one hour
  2. concentrationThe reaction solution was concentrated under reduced pressure
  3. dissolutionthe residue was dissolved in water
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with water
  6. dry with materiala saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customto remove the solvent
  9. customThe residue was purified by silica gel column chromatography (eluent; chloroform:methanol=10:1)
  10. additionthe fractions containing the desired compound
  11. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-1f2a53f529d846e88928e0569a00cb58
出典データセット
uspto-grants-1998_12
特許番号
US05847159

反応ノート

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