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

HRID 44743
ノート
印刷プレビュー

反応式

HRID 44743 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 84189Ethoxyacetyl chloride3 回HCID 574578221-{[(3-Amino[1,5]naphthyridin-4-yl)amino]methyl}cyclohexanol

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-933a8fc2b79048d6b1d802bb2795b392
出典データセット
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08541438B2

反応ノート

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