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Dimethylformamide → HCID 76282787, Verbindung

HRID 2199786
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2199786
[NH2:1][C@@H:2]1[CH2:7][CH2:6][CH2:5][N:4]([C:8]2[S:9][C:10]([NH:16][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][N:18]=3)=[C:11]([C:13]([NH2:15])=[O:14])[N:12]=2)[CH2:3]1.CN(C)C=O.C(N(C(C)C)CC)(C)C.[CH3:37][S:38](Cl)(=[O:40])=[O:39]>O1CCCC1>[CH3:37][S:38]([NH:1][C@@H:2]1[CH2:7][CH2:6][CH2:5][N:4]([C:8]2[S:9][C:10]([NH:16][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][N:18]=3)=[C:11]([C:13]([NH2:15])=[O:14])[N:12]=2)[CH2:3]1)(=[O:40])=[O:39]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 6228DimethylformamideHCID 31297Methanesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 90220400HCID 90220400, Verbindung

Produkt 1

HCID 76282787HCID 76282787, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028
Tetrahydrofuran
Lösungsmittel

Versuchsvorschrift

To a suspension of 2-((R)-3-amino-piperidin-1-yl)-5-(pyridin-2-ylamino)-thiazole-4-carboxylic acid amide (prepared as described in example 4) (5.6 mg, 171 μmol) in tetrahydrofuran (1 mL) was added N,N-dimethylformamide (0.5 mL) to form a clear solution. Diisopropylethylamine (59.9 μL, 343 μmol) was added followed by methanesulfonyl chloride (20 μL, 257 μmol) and the mixture left to stir overnight at ambient temperature under argon. The reaction mixture was quenched by the addition of saturated aqueous ammonium chloride solution (2 mL), poured into water (5 mL) and extracted with ethyl acetate (5×2 mL), the combined organic extracts were washed with brine (2×2 mL), dried over sodium sulfate, filtered and concentrated in vacuo. The residue was purified by reverse phase chromatography using a C-18 column gradient eluted from 10% acetonitrile in water to 100% acetonitrile. The product containing fractions were combined and concentrated in vacuo. The residue was lyophilized from water/ethanol to give (R)-2-(3-(methylsulfonamido)piperidin-1-yl)-5-(pyridin-2-ylamino)thiazole-4-carboxamide as an off-white lyophilized powder (41 mg, 60%).

Aufarbeitung

  1. customto form a clear solution
  2. waitthe mixture left
  3. customThe reaction mixture was quenched by the addition of saturated aqueous ammonium chloride solution (2 mL)
  4. additionpoured into water (5 mL)
  5. extractionextracted with ethyl acetate (5×2 mL)
  6. washthe combined organic extracts were washed with brine (2×2 mL)
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo
  10. customThe residue was purified by reverse phase chromatography
  11. washeluted from 10% acetonitrile in water to 100% acetonitrile
  12. additionThe product containing fractions
  13. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-efe36e784e7749d1b2a90a43362f9cfc
Quelldatensatz
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09359345B2

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