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Lithium hydroxide, monohydrate → HCID 57991948, Verbindung

HRID 2075390
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2075390
[F:1][C:2]1[N:3]=[CH:4][C:5]2[C:10]([CH:11]=1)=[CH:9][C:8]([C:12]([O:14]C)=[O:13])=[CH:7][CH:6]=2.O.[OH-].[Li+]>C1COCC1.CO.O>[F:1][C:2]1[N:3]=[CH:4][C:5]2[C:10]([CH:11]=1)=[CH:9][C:8]([C:12]([OH:14])=[O:13])=[CH:7][CH:6]=2
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Komponenten

4

Edukt 2

HCID 168937Lithium hydroxide, monohydrateHCID 67089276HCID 67089276, Verbindung

Produkt 1

HCID 57991948HCID 57991948, VerbindungAusbeute 468,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 21892291Methanol tetrahydrofuran waterLösungsmittel

Versuchsvorschrift

A mixture of methyl 3-fluoroisoquinoline-6-carboxylate (0.257 g, 1.25 mmol) and lithium hydroxide, monohydrate (105 mg, 2.51 mmol) in THF:MeOH:H2O (3:2:1, 4 mL) was stirred at room temperature for 3 hours. The MeOH and THF were evaporated. 5% citric acid was added, and the mixture was further acidified to pH=4 with NaHSO4. The precipitate was recovered by filtration. The filtrate was extracted with chloroform-isopropanol. The organic extracts were washed with water, brine, dried over sodium sulfate and evaporated. The solids were combined to provide the product as a white solid (1.12 g, 100%). LCMS (API-ES) m/z: 192 (M+H+).

Aufarbeitung

  1. customThe MeOH and THF were evaporated
  2. addition5% citric acid was added
  3. filtrationThe precipitate was recovered by filtration
  4. extractionThe filtrate was extracted with chloroform-isopropanol
  5. washThe organic extracts were washed with water, brine
  6. dry with materialdried over sodium sulfate
  7. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-a2984d84c2a94b6f8c887b93ab2a4227
Quelldatensatz
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07919504B2

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