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

HRID 44686
ノート
印刷プレビュー

反応式

HRID 44686 の反応式
[N+:1]([C:4]1[CH:5]=[N:6][C:7]2[C:12]([C:13]=1[NH:14][CH2:15][C:16]1([OH:22])[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1)=[CH:11][CH:10]=[CH:9][CH:8]=2)([O-])=O.C(N(CC)CC)C.[CH2:30]([O:32][CH2:33][C:34](Cl)=O)[CH3:31]>[Pt].C1(C)C=CC=CC=1.C(O)C>[CH2:30]([O:32][CH2:33][C:34]1[N:14]([CH2:15][C:16]2([OH:22])[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]2)[C:13]2[C:12]3[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=3[N:6]=[CH:5][C:4]=2[N:1]=1)[CH3:31]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 8471TriethylamineHCID 84189Ethoxyacetyl chlorideHCID 574578081-[(3-Nitroquinolin-4-ylamino)methyl]cyclohexanol

生成物 1

HCID 575153771-{[2-(ethoxymethyl)-1H-imidazo[4,5-c]quinolin-1-yl]methyl}cyclohexanol

試薬・触媒・溶媒 3

HCID 23939Platinum触媒HCID 702Ethanol
溶媒
HCID 1140Toluene溶媒

実験手順

A mixture of the 1-{[(3-nitroquinolin-4-yl)amino]methyl}cyclohexanol prepared above (87%, 7.00 g, 20.3 mmol) and 5% platinum on carbon (0.60 g) in toluene (160 mL) and ethanol (20 mL) was hydrogenated at 20-30 psi (1.4×105 to 2.1×105 Pa) on a Parr apparatus for 2 h. The mixture was filtered through CELITE filter agent, which was rinsed with toluene. The filtrate was concentrated to a golden oil. The oil was concentrated twice from toluene. To the oil was added CH2Cl2 (200 mL) and the resulting solution was cooled in an ice bath. Triethylamine (3.11 mL, 22.3 mmol) was added followed by dropwise addition of ethoxyacetyl chloride (88%, 2.96 g, 21.3 mmol). The solution was allowed to warm to rt and stir for 1 h, during which time a precipitate formed. The reaction mixture was concentrated to a yellow foam to which ethanol (200 mL) and triethylamine (11 mL) were added. The resulting solution was heated at reflux for 13 h. The solution was concentrated to a yellow solid, which was dissolved in CH2Cl2 (150 mL) and washed with water (50 mL) and brine (75 mL). The organic layer was dried over MgSO4, filtered, and concentrated to a solid that was crystallized from CDCl3/CH2Cl2 to yield 1-{[2-(ethoxymethyl)-1H-imidazo[4,5-c]quinolin-1-yl]methyl}cyclohexanol as pale orange crystals after drying (1.94 g, 28%).

後処理

  1. filtrationThe mixture was filtered through CELITE
  2. filtrationfilter agent, which
  3. washwas rinsed with toluene
  4. concentrationThe filtrate was concentrated to a golden oil
  5. concentrationThe oil was concentrated twice from toluene
  6. additionTo the oil was added CH2Cl2 (200 mL)
  7. temperaturethe resulting solution was cooled in an ice bath
  8. customformed
  9. concentrationThe reaction mixture was concentrated to a yellow foam to which ethanol (200 mL) and triethylamine (11 mL)
  10. additionwere added
  11. temperatureThe resulting solution was heated
  12. temperatureat reflux for 13 h
  13. concentrationThe solution was concentrated to a yellow solid, which
  14. dissolutionwas dissolved in CH2Cl2 (150 mL)
  15. washwashed with water (50 mL) and brine (75 mL)
  16. dry with materialThe organic layer was dried over MgSO4
  17. filtrationfiltered
  18. concentrationconcentrated to a solid
  19. customthat was crystallized from CDCl3/CH2Cl2

出典と根拠

ORDレコード
ord-b8bd5dff2a7343c09be846ff0af6e98c
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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