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Benzoyl chloride → 7-[1-(Pyridin-4-yl)piperidin-4-ylmethoxy]-1,2,3,4-tetrahydroisoquinoline-2-carbothioamide

HRID 412516
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HRID 412516 반응식
[N-:1]=[C:2]=[S:3].[NH4+].C(Cl)(=O)C1C=CC=CC=1.[N:14]1[CH:19]=[CH:18][C:17]([N:20]2[CH2:25][CH2:24][CH:23]([CH2:26][O:27][C:28]3[CH:37]=[C:36]4[C:31]([CH2:32][CH2:33][NH:34][CH2:35]4)=[CH:30][CH:29]=3)[CH2:22][CH2:21]2)=[CH:16][CH:15]=1>CC(C)=O.C(Cl)Cl>[N:14]1[CH:19]=[CH:18][C:17]([N:20]2[CH2:21][CH2:22][CH:23]([CH2:26][O:27][C:28]3[CH:37]=[C:36]4[C:31]([CH2:32][CH2:33][N:34]([C:2](=[S:3])[NH2:1])[CH2:35]4)=[CH:30][CH:29]=3)[CH2:24][CH2:25]2)=[CH:16][CH:15]=1
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참가 물질

6

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HCID 7412Benzoyl chlorideHCID 113247627-[1-(Pyridin-4-yl)piperidin-4-ylmethoxy]-1,2,3,4-tetrahydroisoquinolineHCID 178514171HCID 178514171, 화합물

생성물 1

HCID 185363907-[1-(Pyridin-4-yl)piperidin-4-ylmethoxy]-1,2,3,4-tetrahydroisoquinoline-2-carbothioamide수율 44.8%

시약·촉매·용매 2

HCID 180Acetone용매2회
HCID 6344Dichloromethane용매

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온도
75 °C

실험 절차

To a solution of ammonium isothiocyanate (220 mg) in acetone (4.5 ml) was dropwise added benzoyl chloride (0.32 ml) at room temperature, and the mixture was stirred at 75° C. for 10 min. Then, a mixture of 7-[1-(pyridin-4-yl)piperidin-4-ylmethoxy]-1,2,3,4-tetrahydroisoquinoline (850 mg) in acetone (4.5 ml) and methylene chloride (4.5 ml) was added dropwise, and the mixture was stirred at the same temperature for 1 hour. After completion of the reaction, the solvent was evaporated and water was added. The mixture was extracted with chloroform. The organic layer was washed successively with water and saturated brine and dried over anhydrous sodium sulfate, and the solvent was evaporated. To the obtained residue was added conc. hydrochloric acid (10 ml), and the mixture was stirred under reflux for 1 hour. After completion of the reaction, water was added and the mixture was washed successively with ethyl acetate and chloroform. The aqueous layer was concentrated and the resultant residue was dissolved in water and ethanol, and neutralized with ion-exchange resin (IRA-410). This was filtrated and the filtrate was concentrated. The obtained residue was purified by silica gel column chromatography (chloroform:methanol=100:1-20:1) and dried under reduced pressure to give the title compound (450 mg).

후처리

  1. customat room temperature
  2. additionwas added dropwise
  3. stirringthe mixture was stirred at the same temperature for 1 hour
  4. customAfter completion of the reaction
  5. customthe solvent was evaporated
  6. additionwater was added
  7. extractionThe mixture was extracted with chloroform
  8. washThe organic layer was washed successively with water and saturated brine
  9. dry with materialdried over anhydrous sodium sulfate
  10. customthe solvent was evaporated
  11. additionTo the obtained residue was added conc. hydrochloric acid (10 ml)
  12. stirringthe mixture was stirred
  13. temperatureunder reflux for 1 hour
  14. customAfter completion of the reaction, water
  15. additionwas added
  16. washthe mixture was washed successively with ethyl acetate and chloroform
  17. concentrationThe aqueous layer was concentrated
  18. dissolutionthe resultant residue was dissolved in water
  19. filtrationThis was filtrated
  20. concentrationthe filtrate was concentrated
  21. customThe obtained residue was purified by silica gel column chromatography (chloroform:methanol=100:1-20:1)
  22. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-0214daebda06404b81258dbf5b9f6c6a
출처 데이터셋
uspto-grants-2003_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06562828B1

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