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Aldoxime → 4-chloro-2-(ethoxymethyl)-1-[2-(3-methyl-1-oxa-2,4-diazaspiro[4,4]non-2-en-4-yl)ethyl]-1H-imidazo[4,5-c]quinoline

HRID 606084
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Reaktionsgleichung

Reaktionsgleichung von HRID 606084
[Cl:1][C:2]1[C:11]2[N:12]=[C:13]([CH2:18][O:19][CH2:20][CH3:21])[N:14]([CH2:15][CH2:16][NH2:17])[C:10]=2[C:9]2[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=2[N:3]=1.[C:22]1(=[O:27])[CH2:26][CH2:25][CH2:24][CH2:23]1.S([O-])([O-])(=O)=O.[Mg+2].[CH:34](=[N:36]O)[CH3:35].ClN1C(=O)CCC1=O.C(N(CC)CC)C>ClCCl>[Cl:1][C:2]1[C:11]2[N:12]=[C:13]([CH2:18][O:19][CH2:20][CH3:21])[N:14]([CH2:15][CH2:16][N:17]3[C:22]4([CH2:26][CH2:25][CH2:24][CH2:23]4)[O:27][N:36]=[C:34]3[CH3:35])[C:10]=2[C:9]2[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=2[N:3]=1
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Komponenten

8

Edukt 6

HCID 7863AldoximeHCID 8452CyclopentanoneHCID 8471TriethylamineHCID 24083Sulfuric acid magnesium salt (1:1)HCID 31398ChlorosuccinimideHCID 862476222-(4-chloro-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-1-yl)ethylamine

Produkt 1

HCID 86616887
4-chloro-2-(ethoxymethyl)-1-[2-(3-methyl-1-oxa-2,4-diazaspiro[4,4]non-2-en-4-yl)ethyl]-1H-imidazo[4,5-c]quinoline
Ausbeute 54,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture of 2-(4-chloro-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-1-yl)ethylamine (1.00 g, 3.28 mmol), cyclopentanone (0.32 mL, 3.6 mmol), and magnesium sulfate in dichloromethane was stirred at room temperature overnight. The mixture was filtered and the filtrate was concentrated under reduced pressure. The residue was dissolved in dichloromethane (20 mL) along with N-hydroxyethanimidoyl chloride, which was prepared from acetaldehyde oxime (242 mg, 4.10 mmol) and N-chlorosuccinimide (537 mg, 4.10 mmol) according to the method described in Part G of Example 10. The resulting solution was cooled in an ice bath and triethylamine (0.69 mL, 4.9 mmol) was added. The mixture was allowed to warm slowly to room temperature and stirred overnight. The work-up and purification procedures described in Part G of Example 10 were followed to provide 770 mg of 4-chloro-2-(ethoxymethyl)-1-[2-(3-methyl-1-oxa-2,4-diazaspiro[4,4]non-2-en-4-yl)ethyl]-1H-imidazo[4,5-c]quinoline as a clear, colorless oil.

Aufarbeitung

  1. filtrationThe mixture was filtered
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. dissolutionThe residue was dissolved in dichloromethane (20 mL) along with N-hydroxyethanimidoyl chloride, which
  4. temperatureThe resulting solution was cooled in an ice bath
  5. temperatureto warm slowly to room temperature
  6. stirringstirred overnight
  7. customThe work-up and purification procedures

Quellen und Nachweise

ORD-Eintrag
ord-70ff8d3d1cae4c6dbf645630c8096baa
Quelldatensatz
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07915281B2

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