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Ammonium Chloride → 6-(7-hydroxy-6,7-dihydro-5H-pyrrolo[1,2-c]imidazol-7-yl)-N-methyl-2-naphthamide

HRID 420218
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HRID 420218 반응식
C(N(C(C)C)CC)(C)C.[OH:10][C:11]([C:39]1[CH:40]=[C:41]2[C:46](=[CH:47][CH:48]=1)[CH:45]=[C:44]([C:49]([NH:51][CH3:52])=[O:50])[CH:43]=[CH:42]2)([C:15]1[N:16]=[CH:17][N:18](C(C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[CH:19]=1)[CH2:12][CH2:13]O.CS(Cl)(=O)=O.[Cl-].[NH4+]>C(OCC)(=O)C.CO.O.CS(C)=O.C1COCC1>[OH:10][C:11]1([C:39]2[CH:40]=[C:41]3[C:46](=[CH:47][CH:48]=2)[CH:45]=[C:44]([C:49]([NH:51][CH3:52])=[O:50])[CH:43]=[CH:42]3)[C:15]2[N:16]([CH:17]=[N:18][CH:19]=2)[CH2:13][CH2:12]1
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참가 물질

10

반응물 4

HCID 25517Ammonium ChlorideHCID 31297Methanesulfonyl chloride2회HCID 81531Diisopropylethylamine3회HCID 101530586-[1,3-dihydroxy-1-(1-trityl-1H-imidazol-4-yl)propyl]-N-methyl-2-naphthamide

생성물 1

HCID 98830296-(7-hydroxy-6,7-dihydro-5H-pyrrolo[1,2-c]imidazol-7-yl)-N-methyl-2-naphthamide수율 80%

시약·촉매·용매

5
HCID 679Dimethyl Sulfoxide용매HCID 887Methanol용매HCID 962Water용매HCID 8028Tetrahydrofuran용매2회HCID 8857Ethyl Acetate용매

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온도
25 °C

실험 절차

20 mL of THF and 1.23 mL (3.14 mmol, 2 eq) of diisopropylethylamine were added to 2 g (3.523 mmol) of 6-[1,3-dihydroxy-1-(1-trityl-1H-imidazol-4-yl)propyl]-N-methyl-2-naphtamide. 20 mL of THF was further added. 0.35 mL (4.58 mmol, 1.3 eq) of methylsulfonyl chloride was added dropwise at 2˜3° C., and the mixture was stirred at 2˜3° C. for 25 minutes. 16 mL of dimethyl sulfoxide was added dropwise at 2˜3° C., and the mixture was stirred at 0˜3° C. for 45 minutes. 0.2 mL of methylsulfonyl chloride and 0.5 mL of diisopropylethylamine were added at 0˜3° C., and the mixture was stirred at 0˜3° C. for 20 minutes. 4 mL of water was added dropwise at 0˜8° C., and the layers were separated. The aqueous layer was re-extracted with 10 mL of ethyl acetate two times, the organic layers were combined, and washed with 4 mL of an aqueous saturated sodium chloride solution two times. The material was dried with magnesium sulfate, and concentrated under reduced pressure. The concentration residue was dissolved in 15 mL of acetonitrile, and the solution was stirred at 60˜63° C. for 20 minutes. To the reaction solution were added 4.5 mL of methanol and 1.23 mL (3.14 mmol, 2 eq) of diisopropylethylamine. The mixture was stirred at 60˜63° C. for 2 hours. After cooled to 25° C., 30 mL of an aqueous saturated ammonium chloride solution and 40 mL of ethyl acetate were added, and the layers were separated. The organic layer was back extracted with 10 mL of 0.5N hydrochloric acid-aqueous saturated ammonium chloride solution. The aqueous layers were combined, a pH was adjusted to 8 with a 30% aqueous sodium hydroxide solution, followed by stirring at 25° C. for 18 hours and 15 minutes, and at 0˜5° C. for 1 hour and 25 minutes. Crystals were filtered, and washed with water. Vacuum drying (50° C.) to a constant weight afforded 0.87 g. of 6-[7-hydroxy-6,7-dihydro-5H-pyrrolo[1,2-c]imidazol-7-yl]-N-methyl-2-naphthamide (yield 80%).

후처리

  1. stirringthe mixture was stirred at 0˜3° C. for 45 minutes
  2. stirringthe mixture was stirred at 0˜3° C. for 20 minutes
  3. customthe layers were separated
  4. extractionThe aqueous layer was re-extracted with 10 mL of ethyl acetate two times
  5. washwashed with 4 mL of an aqueous saturated sodium chloride solution two times
  6. dry with materialThe material was dried with magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. dissolutionThe concentration residue was dissolved in 15 mL of acetonitrile
  9. stirringthe solution was stirred at 60˜63° C. for 20 minutes
  10. stirringThe mixture was stirred at 60˜63° C. for 2 hours
  11. customthe layers were separated
  12. extractionThe organic layer was back extracted with 10 mL of 0.5N hydrochloric acid-aqueous saturated ammonium chloride solution
  13. stirringby stirring at 25° C. for 18 hours and 15 minutes
  14. waitat 0˜5° C. for 1 hour
  15. custom25 minutes
  16. filtrationCrystals were filtered
  17. washwashed with water
  18. customVacuum drying (50° C.) to a constant weight
  19. customafforded 0.87 g

출처 및 근거

ORD 기록
ord-2bc5ec79904b4aa9a5ff59e688671a56
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08093403B2

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