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Methanol → N-Cyclopropyl-4-methyl-3-[1-oxo-7-(piperidin-4-yloxy)isoquinolin-2(1H)-yl]benzamide

HRID 506979
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 506979
[CH:1]1([NH:4][C:5](=[O:25])[C:6]2[CH:11]=[CH:10][C:9]([CH3:12])=[C:8]([N:13]3[CH:22]=[CH:21][C:20]4[C:15](=[CH:16][C:17]([OH:23])=[CH:18][CH:19]=4)[C:14]3=[O:24])[CH:7]=2)[CH2:3][CH2:2]1.[F-].[Cs+].C(OC([N:35]1[CH2:40][CH2:39][CH:38](OS(C)(=O)=O)[CH2:37][CH2:36]1)=O)(C)(C)C.CO>CC(N(C)C)=O.C(OCC)(=O)C.Cl.O1CCOCC1>[CH:1]1([NH:4][C:5](=[O:25])[C:6]2[CH:11]=[CH:10][C:9]([CH3:12])=[C:8]([N:13]3[CH:22]=[CH:21][C:20]4[C:15](=[CH:16][C:17]([O:23][CH:38]5[CH2:39][CH2:40][NH:35][CH2:36][CH2:37]5)=[CH:18][CH:19]=4)[C:14]3=[O:24])[CH:7]=2)[CH2:3][CH2:2]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 4

HCID 887MethanolHCID 25953Cesium fluorideHCID 41848691-(tert-Butoxycarbonyl)-4-(methanesulfonyloxy)piperidine2×HCID 11515516N-Cyclopropyl-3-(7-hydroxy-1-oxoisoquinolin-2(1H)-yl)-4-methylbenzamide

Produkt 1

HCID 67018601N-Cyclopropyl-4-methyl-3-[1-oxo-7-(piperidin-4-yloxy)isoquinolin-2(1H)-yl]benzamide

Reagenzien, Katalysatoren, Lösungsmittel

4
HCID 313Hydrochloric AcidLösungsmittelHCID 8857Ethyl AcetateLösungsmittelHCID 312751,4-DioxaneLösungsmittelHCID 31374DimethylacetamideLösungsmittel

Versuchsvorschrift

N-Cyclopropyl-3-(7-hydroxy-1-oxoisoquinolin-2(1H)-yl)-4-methylbenzamide (200 mg) was stirred with cesium fluoride (364 mg) and 4-methanesulfonyloxypiperidine-1-carboxylic acid tert-butyl ester (251 mg) in DMA (1.5 ml) at 85° C. for 24 hours (during this time further additions (4×125 mg) of 4-methanesulfonyloxypiperidine-1-carboxylic acid tert-butyl ester took place). The reaction mixture was diluted with ethyl acetate and washed with 1N NaOH (2×), water (3×), brine, dried (magnesium sulfate) and concentrated to a brown oil. Purification by column chromatography with a gradient of 50% ethyl acetate/iso-hexane to 100% ethyl acetate gave a cream coloured solid. The solid was dissolved in 4M HCl in dioxane solution (1 ml) and methanol (0.5 ml) and stirred for 16 hours at room temperature. The reaction mixture was concentrated and the residue was purified by column chromatography on an ion exchange column (isolute SCX column from International Sorbent Technology Limited, Henoed, Mid-Glamorgan, UK) using initially methanol and then a 99:1 mixture of methanol and aqueous ammonia solution to give N-cyclopropyl-4-methyl-3-[1-oxo-7-(piperidin-4-yloxy)isoquinolin-2(1H)-yl]benzamide as a cream coloured foam solid (146 mg); NMR Spectrum: (DMSOd6) 0.55 (m, 2H), 0.69 (m, 2H), 1.50 (m, 2H), 1.95 (m, 2H), 2.10 (s, 3H), 2.60 (m, 2H), 2.84 (m, 1H), 2.96 (m, 2H), 4.54 (m, 1H), 6.71 (d, 1H), 7.20 (d, 1H), 7.41 (d, 1H), 7.49 (d, 1H), 7.67 (s, 1H), 7.80 (d, 1H), 7.83 (s, 1H), 7.87 (d, 1H), 8.42 (d, 1H); Mass Spectrum: M+H+ 418.

Aufarbeitung

  1. washwashed with 1N NaOH (2×), water (3×), brine
  2. dry with materialdried (magnesium sulfate)
  3. concentrationconcentrated to a brown oil
  4. customPurification by column chromatography with a gradient of 50% ethyl acetate/iso-hexane to 100% ethyl acetate
  5. customgave a cream
  6. concentrationThe reaction mixture was concentrated
  7. customthe residue was purified by column chromatography on an ion exchange column (isolute SCX column from International Sorbent Technology Limited, Henoed, Mid-Glamorgan, UK)
  8. additiona 99:1 mixture of methanol and aqueous ammonia solution

Quellen und Nachweise

ORD-Eintrag
ord-2970d222f0aa46cfa4c22a2d6d8ec963
Quelldatensatz
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07786115B2

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