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

HRID 922722
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HRID 922722 반응식
O[C@@:2]([C:11]1[CH:12]=[C:13]2[C:18](=[CH:19][CH:20]=1)[CH:17]=[C:16]([C:21]([NH:23][CH3:24])=[O:22])[CH:15]=[CH:14]2)([C:6]1[N:7]=[CH:8][NH:9][CH:10]=1)[CH2:3][CH2:4]O.C(N(C(C)C)C(C)C)C.CS(Cl)(=O)=[O:36].C(=O)([O-])[O-].[Na+].[Na+]>O1CCCC1.O.C(OCC)(=O)C>[OH:36][C:10]1[N:9]=[CH:8][N:7]2[CH2:4][CH2:3][C@@H:2]([C:11]3[CH:12]=[C:13]4[C:18](=[CH:19][CH:20]=3)[CH:17]=[C:16]([C:21]([NH:23][CH3:24])=[O:22])[CH:15]=[CH:14]4)[C:6]=12
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참가 물질

8

반응물 4

HCID 10340Sodium CarbonateHCID 31297Methanesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 178485275HCID 178485275, 화합물

생성물 1

HCID 666510376-((7S)-hydroxy-6,7-dihydro-5H-pyrrolo[1,2-c]imidazol-7-yl)-N-methyl-2-naphthamide수율 58.1%

시약·촉매·용매 3

HCID 962
Water
용매
HCID 8028Tetrahydrofuran용매
HCID 8857Ethyl Acetate용매

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온도
60 °C

실험 절차

To a solution of 6-[(1S)-1,3-dihydroxy-1-(1H-imidazol-4-yl)propyl]-N-methyl-2-naphthamide (1.0 g, 3.1 mmol) in tetrahydrofuran (100 mL) were added N-ethyldiisopropylamine (2.39 g, 18.4 mmol) and methanesulfonyl chloride (2.11 g, 18.4 mmol) at room temperature. The mixture was stirred at the same temperature for 3 hr. To the reaction mixture was added a solution of sodium carbonate (1.31 g, 12.3 mmol) in water (3 mL). The mixture was heated to 60° C. and stirred for 5 hr. After the reaction mixture was allowed to cool to room temperature, ethyl acetate (25 mL) was added thereto. The organic layer was separated and concentrated under reduced pressure. Methanol (16.7 mL) and water (6.4 mL) were added to the residue. The mixture was heated to 65° C., and activated carbon (45 mg) was added thereto. After stirring at the same temperature for 30 min, the activated carbon was filtered off and washed with methanol (1.1 mL). Water (6.4 mL) was added to the filtrate at 55° C. The resulting mixture was allowed to cool to room temperature and stirred for 30 min. To the mixture was added water (6.4 mL) at the same temperature, and the mixture was stirred for 2 hr. The mixture was cooled to 0° C. and stirred for 2 hr. The obtained precipitated crystals were collected by filtration, washed with 45% aqueous methanol (3 mL), and dried under reduced pressure to give 6-((7S)-hydroxy-6,7-dihydro-5H-pyrrolo[1,2-c]imidazol-7-yl)-N-methyl-2-naphthamide (540 mg, 1.8 mmol). yield 57%.

후처리

  1. stirringstirred for 5 hr
  2. temperatureto cool to room temperature
  3. customThe organic layer was separated
  4. concentrationconcentrated under reduced pressure
  5. additionMethanol (16.7 mL) and water (6.4 mL) were added to the residue
  6. temperatureThe mixture was heated to 65° C.
  7. additionactivated carbon (45 mg) was added
  8. stirringAfter stirring at the same temperature for 30 min
  9. filtrationthe activated carbon was filtered off
  10. washwashed with methanol (1.1 mL)
  11. additionWater (6.4 mL) was added to the filtrate at 55° C
  12. temperatureto cool to room temperature
  13. stirringstirred for 30 min
  14. additionTo the mixture was added water (6.4 mL) at the same temperature
  15. stirringthe mixture was stirred for 2 hr
  16. temperatureThe mixture was cooled to 0° C.
  17. stirringstirred for 2 hr
  18. customThe obtained precipitated crystals
  19. filtrationwere collected by filtration
  20. washwashed with 45% aqueous methanol (3 mL)
  21. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-788ea0540b284ec39b05d755f95197ba
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09278938B2

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