HCID 11043960, 화합물 → AH-9700 free base

HRID 1457313노트

반응식

HRID 1457313 반응식
[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

참가 물질

4

반응물 1

HCID 11043960HCID 11043960, 화합물

생성물 1

HCID 9816524AH-9700 free base수율 64.7%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1f2a53f529d846e88928e0569a00cb58
출처 데이터셋
uspto-grants-1998_12
특허 번호
US05847159

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