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Trifluoroacetic acid → 6-(adamantan-1-ylmethoxy)-5-cyclopropyl-N-(N-methylsulfamoyl)nicotinamide

HRID 1849697
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1849697
[C:1]12([CH2:11][O:12][C:13]3[C:25]([CH:26]4[CH2:28][CH2:27]4)=[CH:24][C:16]([C:17](OC(C)(C)C)=[O:18])=[CH:15][N:14]=3)[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[CH2:2]1)[CH2:8]2.FC(F)(F)C(O)=O.C(C1NC=CN=1)(C1NC=CN=1)=O.[CH3:48][NH:49][S:50]([NH2:53])(=[O:52])=[O:51].N1(C2CCCCCCCCCC2)CCCN=CCCCCC1>ClCCl.C(OCC)(=O)C>[C:1]12([CH2:11][O:12][C:13]3[C:25]([CH:26]4[CH2:28][CH2:27]4)=[CH:24][C:16]([C:17]([NH:53][S:50](=[O:52])(=[O:51])[NH:49][CH3:48])=[O:18])=[CH:15][N:14]=3)[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[CH2:2]1)[CH2:8]2
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 6422Trifluoroacetic acidHCID 5250894Bis-(1H-imidazol-2-YL)-methanoneHCID 13168287(Methylsulfamoyl)amineHCID 86703569Tert-butyl 6-(adamantan-1-ylmethoxy)-5-cyclopropylnicotinateHCID 1296629601,8-Diazabicycloundec-7ene

Produkt 1

HCID 86703568
6-(adamantan-1-ylmethoxy)-5-cyclopropyl-N-(N-methylsulfamoyl)nicotinamide
Ausbeute 22 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6344DichloromethaneLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

A solution of tert-butyl 6-(adamantan-1-ylmethoxy)-5-cyclopropylnicotinate (0.50 g, 1.30 mmol) in dichloromethane (20 mL) was treated with trifluoroacetic acid (5.0 mL). The resulting mixture was stirred for 30 minutes and then concentrated in vacuo. The residue was treated with methanol (20 mL) and concentrated in vacuo. The residue was dissolved in anhydrous tetrahydrofuran (20 mL), treated with carbonyl diimidazole (0.42 g, 2.60 mmol), and refluxed under nitrogen for 30 min. The reaction mixture was cooled to ambient temperature and added (methylsulfamoyl)amine (0.43 g, 3.90 mmol) and 1,8-diazabicycloundec-7-ene (0.58 mL, 3.90 mmol). The reaction mixture was refluxed under nitrogen for 30 minutes. The reaction mixture was cooled to ambient temperature, diluted with ethyl acetate (50 mL), washed with 1 M aqueous hydrochloric acid solution (2×30 mL) and brine (30 mL); dried over anhydrous sodium sulfate; filtered and concentrated in vacuo. The residue was purified by silica gel column chromatography (2:1 hexanes:ethyl acetate (+0.2% acetic acid v/v)) to provide the title compound (0.12 g, 22%): 1H NMR (300 MHz, DMSO-d6) δ 11.65 (br s, 1H), 8.46 (d, J=2.3 Hz, 1H), 7.73 (d, J=2.3 Hz, 1H), 7.58-7.51 (m, 1H), 3.92 (s, 2H), 2.52-2.48 (m, 3H), 2.07-1.98 (m, 1H), 1.97-1.90 (m, 3H), 1.72-1.55 (m, 12H), 0.98-0.90 (m, 2H), 0.77-0.70 (m, 2H); MS (ES+) m/z 420.2 (M+1).

Aufarbeitung

  1. concentrationconcentrated in vacuo
  2. additionThe residue was treated with methanol (20 mL)
  3. concentrationconcentrated in vacuo
  4. dissolutionThe residue was dissolved in anhydrous tetrahydrofuran (20 mL)
  5. temperaturerefluxed under nitrogen for 30 min
  6. temperatureThe reaction mixture was refluxed under nitrogen for 30 minutes
  7. temperatureThe reaction mixture was cooled to ambient temperature
  8. washwashed with 1 M aqueous hydrochloric acid solution (2×30 mL) and brine (30 mL)
  9. dry with materialdried over anhydrous sodium sulfate
  10. filtrationfiltered
  11. concentrationconcentrated in vacuo
  12. customThe residue was purified by silica gel column chromatography (2:1 hexanes

Quellen und Nachweise

ORD-Eintrag
ord-dd6c74f13a9d4a19b4f7c6521d96811c
Quelldatensatz
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08952169B2

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