Lithium Hydroxide → HCID 25744650, Verbindung

HRID 84191Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 84191
[Li+].[OH-].C[O:4][C:5]([C:7]1[CH:8]=[C:9]2[C:13](=[CH:14][CH:15]=1)[N:12]([S:16]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)(=[O:18])=[O:17])[CH2:11][CH2:10]2)=[O:6]>O1CCOCC1>[C:19]1([S:16]([N:12]2[C:13]3[C:9](=[CH:8][C:7]([C:5]([OH:6])=[O:4])=[CH:15][CH:14]=3)[CH2:10][CH2:11]2)(=[O:18])=[O:17])[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1

Komponenten

4

Edukt 2

HCID 3939Lithium HydroxideHCID 31756086Methyl 1-(Phenylsulfonyl)indoline-5-carboxylate

Produkt 1

HCID 25744650HCID 25744650, VerbindungAusbeute 93,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

1M LiOH aqueous solution (2.4 ml, 2.40 mmol) was added to a solution of 11 (0.38 g, 1.20 mmol) in dioxane (15 mL). The reaction mixture was stirred at 40° C. overnight and then was concentrated under reduced pressure. The residue was dissolved in water and concentrated HCl was added up to acidic pH to give the precipitation, which was dried by vacuum to afford 16 (0.34 g). 1H NMR (500 MHz, CD3OD): δ 2.97 (t, J=8.6 Hz, 2H), 3.99 (t, J=8.6 Hz, 2H), 7.51-7.54 (m, 2H), 7.61-7.64 (m, 2H), 7.74 (s, 1H), 7.84-7.88 (m, 3H).

Aufarbeitung

  1. concentrationwas concentrated under reduced pressure
  2. dissolutionThe residue was dissolved in water
  3. additionconcentrated HCl was added up to acidic pH
  4. customto give
  5. customthe precipitation, which
  6. customwas dried by vacuum

Quellen und Nachweise

ORD-Eintrag
ord-b7a24551a1f34319a5084d47e707ac02
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08846748B2

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