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Sodium Hydroxide → 1-{[2-(ethoxymethyl)-1H-imidazo[4,5-c][1,5]naphthyridin-1-yl]methyl}cyclohexanol

HRID 1469284
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HRID 1469284 반응식
[CH2:1]([O:3][CH2:4][C:5](Cl)=O)[CH3:2].[NH2:8][C:9]1[CH:10]=[N:11][C:12]2[C:17]([C:18]=1[NH:19][CH2:20][C:21]1([OH:27])[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]1)=[N:16][CH:15]=[CH:14][CH:13]=2.[OH-].[Na+]>ClCCl>[CH2:1]([O:3][CH2:4][C:5]1[N:19]([CH2:20][C:21]2([OH:27])[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]2)[C:18]2[C:17]3[N:16]=[CH:15][CH:14]=[CH:13][C:12]=3[N:11]=[CH:10][C:9]=2[N:8]=1)[CH3:2]
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참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 84189Ethoxyacetyl chloride3회HCID 574578221-{[(3-Amino[1,5]naphthyridin-4-yl)amino]methyl}cyclohexanol

생성물 1

HCID 575154291-{[2-(ethoxymethyl)-1H-imidazo[4,5-c][1,5]naphthyridin-1-yl]methyl}cyclohexanol수율 76%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Ethoxyacetyl chloride (1.78 g, 14.6 mmol) was added dropwise to a 0° C. solution of 1-{[(3-amino[1,5]naphthyridin-4-yl)amino]methyl}cyclohexanol (prepared as described in Part B of Example 57, 13.2 mmol) in dichloromethane (90 mL). After 1.5 h, more ethoxyacetyl chloride (0.3 mL) was added and stirring was continued for another 30 min. More ethoxyacetyl chloride (0.4 mL) was added and stirring was continued overnight. The solvent was removed under reduced pressure and the residue was dissolved in ethanol (90 mL). Sodium hydroxide (1.06 g, 26.5 mmol) was added and the reaction was heated at reflux for about 1 d. The solvent was removed under reduced pressure and the residue was partitioned between dichloromethane (200 mL) and water (100 mL). The aqueous phase was extracted with dichloromethane (2×100 mL). The combined organic layers were washed with brine (50 mL), dried over MgSO4, filtered, and concentrated under reduced pressure to yield a brown foam. The foam was triturated with ethyl acetate and sonicated briefly. A white solid was isolated by filtration. The filtrate was concentrated and the trituration process was repeated two more times. The off white solids were combined and dried to yield 1-{[2-(ethoxymethyl)-1H-imidazo[4,5-c][1,5]naphthyridin-1-yl]methyl}cyclohexanol (3.40 g, 76% over three steps).

후처리

  1. waitwas continued for another 30 min
  2. stirringstirring
  3. waitwas continued overnight
  4. customThe solvent was removed under reduced pressure
  5. dissolutionthe residue was dissolved in ethanol (90 mL)
  6. temperaturethe reaction was heated
  7. temperatureat reflux for about 1 d
  8. customThe solvent was removed under reduced pressure
  9. customthe residue was partitioned between dichloromethane (200 mL) and water (100 mL)
  10. extractionThe aqueous phase was extracted with dichloromethane (2×100 mL)
  11. washThe combined organic layers were washed with brine (50 mL)
  12. dry with materialdried over MgSO4
  13. filtrationfiltered
  14. concentrationconcentrated under reduced pressure
  15. customto yield a brown foam
  16. customThe foam was triturated with ethyl acetate
  17. customsonicated briefly
  18. customA white solid was isolated by filtration
  19. concentrationThe filtrate was concentrated
  20. customdried

출처 및 근거

ORD 기록
ord-c70852898ad046e5af07eb77edd68ceb
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09006264B2

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