Lithium hydroxide, monohydrate → HCID 59778157, Verbindung

HRID 1363101Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1363101
[CH2:1]([N:8]1[C:17]2[C:12](=[CH:13][C:14]([C:18]([F:21])([F:20])[F:19])=[CH:15][CH:16]=2)[CH2:11][CH:10]([C:22]([O:24]CC)=[O:23])[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.[OH-].[Li+]>CO.C1COCC1.O>[CH2:1]([N:8]1[C:17]2[C:12](=[CH:13][C:14]([C:18]([F:19])([F:20])[F:21])=[CH:15][CH:16]=2)[CH2:11][CH:10]([C:22]([OH:24])=[O:23])[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Komponenten

4

Edukt 2

HCID 168937Lithium hydroxide, monohydrateHCID 59778148HCID 59778148, Verbindung

Produkt 1

HCID 59778157HCID 59778157, VerbindungAusbeute 97 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 21892291Methanol tetrahydrofuran waterLösungsmittel

Versuchsvorschrift

To a solution of 149C (825 mg, 2.27 mmol) in a mixed solvent of MeOH-THF-H2O (20 mL at ratio of 2:2:1) was added lithium hydroxide monohydrate (400 mg, 11.35 mmol). The mixture was stirred at RT for 2 h, then extracted with ether (20 mL). The aqueous layer was acidified to pH 4-5 using 3N aqueous HCl, then extracted with CH2Cl2 (3×). The combined CH2Cl2 extracts were washed with water, brine, dried Na2SO4), and concentrated in vacuo to afford compound 149D as light yellow foam (735 mg, 97%).

Aufarbeitung

  1. extractionextracted with ether (20 mL)
  2. extractionextracted with CH2Cl2 (3×)
  3. washThe combined CH2Cl2 extracts were washed with water, brine, dried Na2SO4), and
  4. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-b70bc25b45da42daa007f4ca22d3de0c
Quelldatensatz
uspto-grants-2011_02
Patentnummer
US07884113B2

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