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Potassium Carbonate → N-((5-((2-(2-(pyrrolidin-1-yl)acetamido)pyridin-4-yl)oxy)pyridin-2-yl)carbamoyl)pivalamide

HRID 626562
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Reaktionsgleichung

Reaktionsgleichung von HRID 626562
[CH2:1]1[CH2:5][N:4]([CH2:6][C:7]([OH:9])=O)[CH2:3][CH2:2]1.S(Cl)(Cl)=O.[NH2:14][C:15]1[CH:20]=[C:19]([O:21][C:22]2[CH:23]=[CH:24][C:25]([NH:28][C:29]([NH:31][C:32](=[O:37])[C:33]([CH3:36])([CH3:35])[CH3:34])=[O:30])=[N:26][CH:27]=2)[CH:18]=[CH:17][N:16]=1.CCN(C(C)C)C(C)C.C([O-])([O-])=O.[K+].[K+]>C(Cl)Cl.C1COCC1>[N:4]1([CH2:6][C:7]([NH:14][C:15]2[CH:20]=[C:19]([O:21][C:22]3[CH:23]=[CH:24][C:25]([NH:28][C:29]([NH:31][C:32](=[O:37])[C:33]([CH3:35])([CH3:34])[CH3:36])=[O:30])=[N:26][CH:27]=3)[CH:18]=[CH:17][N:16]=2)=[O:9])[CH2:3][CH2:2][CH2:1][CH2:5]1
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Komponenten

8

Edukt 5

HCID 11430Potassium CarbonateHCID 24386Thionyl ChlorideHCID 81531DiisopropylethylamineHCID 414564Pyrrolidin-1-ylacetic acidHCID 90409811N-((5-((2-aminopyridin-4-yl)oxy)pyridin-2-yl)carbamoyl)pivalamide

Produkt 1

HCID 86274186
N-((5-((2-(2-(pyrrolidin-1-yl)acetamido)pyridin-4-yl)oxy)pyridin-2-yl)carbamoyl)pivalamide
Ausbeute 15,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6344DichloromethaneLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A solution of 1-pyrrolidinylacetic acid (0.082 g, 0.638 mmol) in thionyl chloride (3 mL, 41.1 mmol) and DCM (3 mL) was stirred at RT for 3 h, concentrated to dryness, suspended in THF (5 mL), added to a 0° C. solution of Example C1 (0.15 g, 0.455 mmol) and DIEA (0.239 mL, 1.366 mmol) in THF (5 mL), allowed to warm to RT and stirred overnight. The mixture was treated with 10% K2CO3, extracted with DCM (4×) and the combined organics were washed with brine, dried over Na2SO4, concentrated to dryness and purified via silica gel chromatography (MeOH/EtOAc). The material was further purified via preparative TLC (MeOH/DCM/TEA) to afford N-((5-((2-(2-(pyrrolidin-1-yl)acetamido)pyridin-4-yl)oxy)pyridin-2-yl)carbamoyl)pivalamide (31 mg, 15%). 1H NMR (400 MHz, DMSO-d6): δ 11.23 (s, 1H), 10.44 (s, 1H), 9.98 (s, 1H), 8.26 (d, J=2.9 Hz, 1H), 8.20 (d, J=5.8 Hz, 1H), 8.09 (d, J=9.0 Hz, 1H), 7.74 (dd, J=9.0, 2.9 Hz, 1H), 7.64 (d, J=2.4 Hz, 1H), 6.74 (dd, J=5.8, 2.4 Hz, 1H), 3.27 (s, 2H), 2.58 (s, 4H), 1.73-1.71 (m, 4H), 1.21 (s, 9H); MS (ESI) m/z: 441.2 (M+H+).

Aufarbeitung

  1. concentrationconcentrated to dryness
  2. extractionextracted with DCM (4×)
  3. washthe combined organics were washed with brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated to dryness
  6. custompurified via silica gel chromatography (MeOH/EtOAc)
  7. customThe material was further purified via preparative TLC (MeOH/DCM/TEA)

Quellen und Nachweise

ORD-Eintrag
ord-d966b9f3bb6f4644a1db04c96882fbfe
Quelldatensatz
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09309224B2

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