Hydrochloric Acid → HCID 178484861, Verbindung

HRID 630376Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 630376
[OH:1][C:2]([C:26]1[S:27][CH:28]=[CH:29][CH:30]=1)([C:21]1[S:22][CH:23]=[CH:24][CH:25]=1)[C:3]([O:5][C@H:6]1[CH2:11][CH2:10][C@H:9]([N:12](C(OC(C)(C)C)=O)[CH3:13])[CH2:8][CH2:7]1)=[O:4].Cl>O1CCOCC1>[OH:1][C:2]([C:21]1[S:22][CH:23]=[CH:24][CH:25]=1)([C:26]1[S:27][CH:28]=[CH:29][CH:30]=1)[C:3]([O:5][C@H:6]1[CH2:7][CH2:8][C@H:9]([NH:12][CH3:13])[CH2:10][CH2:11]1)=[O:4]

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 178486063HCID 178486063, Verbindung2×

Produkt 1

HCID 178484861HCID 178484861, VerbindungAusbeute 78 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel2×

Versuchsvorschrift

To a solution of trans-4-[(tert-butoxycarbonyl)(methyl)amino]cyclohexyl hydroxy(di-2-thienyl)acetate (intermediate 4; 8.1 g, 0.01 mol) in dioxane (13.5 mL) was added hydrogen chloride 4M in dioxane (27 mL). The mixture was stirred at room temperature for 24 hours. The precipitate obtained was filtrated and washed with ether. The crude was dissolved in water and potassium carbonate was added until pH=8-9. The product was extracted with ethyl acetate and the organic layer was washed with brine, dried and evaporated to dryness giving the title compound as a white solid (78%).

Aufarbeitung

  1. customThe precipitate obtained
  2. filtrationwas filtrated
  3. washwashed with ether
  4. dissolutionThe crude was dissolved in water
  5. additionpotassium carbonate was added until pH=8-9
  6. extractionThe product was extracted with ethyl acetate
  7. washthe organic layer was washed with brine
  8. customdried
  9. customevaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-2d8c6416cbac4bb49c7ede0042cd467f
Quelldatensatz
uspto-grants-2016_04
Patentnummer
US09315463B2

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