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Sodium Bicarbonate → (+/-)-2-(cis-2-Fluorocyclohexyl)-5-{[4-(1H-pyrazol-1-yl)phenyl]methyl}-2,5-dihydro-3H-pyrazolo[4,3-c]quinolin-3-one

HRID 341089
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 341089
O[C@@H:2]1[CH2:7][CH2:6][CH2:5][CH2:4][C@H:3]1[N:8]1[C:32](=[O:33])[C:11]2=[CH:12][N:13]([CH2:20][C:21]3[CH:26]=[CH:25][C:24]([N:27]4[CH:31]=[CH:30][CH:29]=[N:28]4)=[CH:23][CH:22]=3)[C:14]3[CH:15]=[CH:16][CH:17]=[CH:18][C:19]=3[C:10]2=[N:9]1.COCCN(S(F)(F)[F:44])CCOC.C(=O)(O)[O-].[Na+]>ClCCl>[F:44][C@H:2]1[CH2:7][CH2:6][CH2:5][CH2:4][C@H:3]1[N:8]1[C:32](=[O:33])[C:11]2=[CH:12][N:13]([CH2:20][C:21]3[CH:26]=[CH:25][C:24]([N:27]4[CH:31]=[CH:30][CH:29]=[N:28]4)=[CH:23][CH:22]=3)[C:14]3[CH:15]=[CH:16][CH:17]=[CH:18][C:19]=3[C:10]2=[N:9]1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 516892Sodium Bicarbonate2×HCID 2734690(Bis(2-methoxyethyl)amino)sulfur trifluoride2×HCID 68154351(+/-)-2-(trans-2-Hydroxycyclohexyl)-5-{[4-(1H-pyrazol-1-yl)phenyl]methyl}-2,5-dihydro-3H-pyrazolo[4,3-c]quinolin-3-one

Produkt 1

HCID 68154082(+/-)-2-(cis-2-Fluorocyclohexyl)-5-{[4-(1H-pyrazol-1-yl)phenyl]methyl}-2,5-dihydro-3H-pyrazolo[4,3-c]quinolin-3-one

Reagenzien, Katalysatoren, Lösungsmittel

1
HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

(±)-2-(trans-2-Hydroxycyclohexyl)-5-{[4-(1H-pyrazol-1-yl)phenyl]methyl}-2,5-dihydro-3H-pyrazolo[4,3-c]quinolin-3-one (Example 508, 0.15 g, 0.35 mmol) was dissolved in dichloromethane (5 mL), cooled to 0° C. and treated with bis(2-methoxyethyl)aminosulfur trifluoride (0.15 mL, 0.70 mmol, 2 equiv). The mixture was stirred at 0° C. for 30 minutes and then treated with additional bis(2-methoxyethyl)aminosulfur trifluoride (75 μL, 0.35 mmol, 1 equiv). After stirring for an additional 30 minutes, the mixture was treated with sodium bicarbonate (5 mL, aqueous saturated) and stirred vigorously for 15 minutes. The mixture was poured into sodium bicarbonate (75 mL, aqueous saturated) and extracted with dichloromethane (2×75 mL). The combined organic extracts were dried with sodium sulfate, filtered and concentrated in vacuo. The residue was purified by silica gel gradient chromatography (100:0 to 85:15; ethyl acetate:methanol), providing the titled compound: 1H-NMR (400 MHz, CDCl3) δ 8.39 (1H, s), 8.38-8.35 (1H, m), 7.89 (1H, d, J=2.5 Hz), 7.71 (1H, d, J=1.8 Hz), 7.69 (2H, d, J=8.6 Hz), 7.47-7.42 (2H, m), 7.40-7.36 (1H, m), 7.28-7.26 (2H, m), 6.46 (1H, dd, J=2.4, 1.8 Hz), 5.45 (2H, s), 5.03 (1H, dtd, J=49.9, 10.6, 5.0 Hz), 4.61-4.52 (1H, m), 2.34-2.27 (1H, m), 2.06-1.98 (2H, m), 1.91-1.80 (2H, m), 1.74-1.59 (1H, m), 1.52-1.43 (2H, m) ppm; high resolution mass spectrometry (ES+) m/z 442.2051 [(M+H)+; calculated for C26H25FN5O: 442.2038].

Aufarbeitung

  1. stirringAfter stirring for an additional 30 minutes
  2. stirringstirred vigorously for 15 minutes
  3. extractionextracted with dichloromethane (2×75 mL)
  4. dry with materialThe combined organic extracts were dried with sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by silica gel gradient chromatography (100:0 to 85:15; ethyl acetate:methanol)

Quellen und Nachweise

ORD-Eintrag
ord-f69241b0869c4338a9a9cc3050754812
Quelldatensatz
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08895580B2

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