Hydrochloric Acid → HCID 178463287, Verbindung

HRID 1912466Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1912466
Cl.O1CCOCC1.CN(C)S([N:13]1[CH:17]=[CH:16][C:15]([C:18]([C:27]2[CH:32]=[CH:31][CH:30]=[C:29]([Cl:33])[CH:28]=2)([NH:20]S(C(C)(C)C)=O)[CH3:19])=[N:14]1)(=O)=O>CO>[Cl:33][C:29]1[CH:28]=[C:27]([C:18]([NH2:20])([C:15]2[CH:16]=[CH:17][NH:13][N:14]=2)[CH3:19])[CH:32]=[CH:31][CH:30]=1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 668253223-[1-(3-Chloro-phenyl)-1-(2-methyl-propane-2-sulfinylamino)-ethyl]-pyrazole-1-sulfonic acid dimethylamide

Produkt 1

HCID 178463287HCID 178463287, VerbindungAusbeute 86 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

Hydrochloric acid 4 M in dioxane (19.79 mL, 79.15 mmol) was added to a solution of 3-[1-(3-chloro-phenyl)-1-(2-methyl-propane-2-sulfinylamino)-ethyl]-pyrazole-1-sulfonic acid dimethylamide (2.29 g, 5.28 mmol) in MeOH (5 mL) and the mixture was stirred at 80° C. in a sealed tube for 18 hours. The solvent was evaporated in vacuo. The residue was poured into NaHCO3 (aq. sat. solution) and extracted with DCM. The organic layer was separated, dried (MgSO4), filtered and the solvents evaporated in vacuo to yield rac-1-(3-chloro-phenyl)-1-(1H-pyrazol-3-yl)-ethylamine (1 g, 86% yield) as a pale yellow solid which was used in the next step without further purification.

Aufarbeitung

  1. customThe solvent was evaporated in vacuo
  2. additionThe residue was poured into NaHCO3 (aq. sat. solution)
  3. extractionextracted with DCM
  4. customThe organic layer was separated
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customthe solvents evaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-89c34f2e4f5040b4a33d7a44b5bcb358
Quelldatensatz
uspto-grants-2013_12
Patentnummer
US08609660B2

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