Sodium Hydroxide → HCID 57436798, Verbindung

HRID 45987Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 45987
[F:1][C:2]([F:25])([F:24])[C:3]1[CH:4]=[C:5]([S:9]([N:12]2[CH2:17][CH2:16][CH2:15][CH2:14][CH:13]2[CH2:18][C:19]([O:21]CC)=[O:20])(=[O:11])=[O:10])[CH:6]=[CH:7][CH:8]=1.[OH-].[Na+]>CO.O1CCOCC1>[F:25][C:2]([F:1])([F:24])[C:3]1[CH:4]=[C:5]([S:9]([N:12]2[CH2:17][CH2:16][CH2:15][CH2:14][CH:13]2[CH2:18][C:19]([OH:21])=[O:20])(=[O:11])=[O:10])[CH:6]=[CH:7][CH:8]=1

Komponenten

5

Edukt 2

HCID 14798Sodium HydroxideHCID 57819731HCID 57819731, Verbindung

Produkt 1

HCID 57436798HCID 57436798, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittel2×HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

The ethyl 2-(1-(3-(trifluoromethyl)phenylsulfonyl)piperidin-2-yl)acetate (10.45 g, 27.5 mmol) was dissolved in a mixture of methanol (150 ml), dioxane (40 ml) and aqueous NaOH solution (4 M, 41.3 ml, 165.2 mmol, 6 eq.) and the solution was stirred overnight When the reaction had ended (TLC control, MC/methanol 95:5), the solution was concentrated. The crude product was taken up in ethyl acetate (600 ml) and the mixture was . . . with KHSO4 solution (0.5 M, 600 ml). The aqueous phase was extracted once more with ethyl acetate (100 ml) and the combined organic phases were washed with sat. NaCl solution (500 ml), dried over Na2SO4 and concentrated. Yield: 9.4 g, 97%.

Aufarbeitung

  1. concentrationthe solution was concentrated
  2. extractionThe aqueous phase was extracted once more with ethyl acetate (100 ml)
  3. washthe combined organic phases were washed with sat. NaCl solution (500 ml)
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-e68a6fb3c19b4a778a2232070437c467
Quelldatensatz
uspto-grants-2013_09
Patentnummer
US08541573B2

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