Hydrochloric Acid → HCID 25052183, Verbindung

HRID 73353Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 73353
C([O:3][C:4](=[O:25])[C:5]1[CH:10]=[CH:9][C:8]([N:11]2[C:19]3[C:14](=[CH:15][C:16]([F:21])=[C:17]([F:20])[CH:18]=3)[C:13]([C:22]#[N:23])=[CH:12]2)=[CH:7][C:6]=1[OH:24])C.O1CCCC1.[OH-].[Li+].Cl>O.C(O)C>[C:22]([C:13]1[C:14]2[C:19](=[CH:18][C:17]([F:20])=[C:16]([F:21])[CH:15]=2)[N:11]([C:8]2[CH:9]=[CH:10][C:5]([C:4]([OH:25])=[O:3])=[C:6]([OH:24])[CH:7]=2)[CH:12]=1)#[N:23]

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 584372264-(3-Cyano-5,6-difluoroindol-1-yl)-2-hydroxybenzoic acid ethyl ester

Produkt 1

HCID 25052183HCID 25052183, VerbindungAusbeute 88,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

To a solution of 4-(3-cyano-5,6-difluoroindol-1-yl)-2-hydroxybenzoic acid ethyl ester (0.074 g) in a mixed solvent of tetrahydrofuran (3.0 mL) and ethanol (0.75 mL) were added 0.1 g/mL aqueous lithium hydroxide solution (0.62 mL) and water (1.0 mL), and this mixture was stirred at room temperature for 26 hours. To this reaction mixture was added 2 mol/L hydrochloric acid (5 mL), this organic solvent was removed under reduced pressure. This resulting mixture was extracted with ethyl acetate, this organic layer was washed with water, and dried over anhydrous magnesium sulfate. The solvent was concentrated under reduced pressure to give the title compounds (0.06 g).

Aufarbeitung

  1. customthis organic solvent was removed under reduced pressure
  2. extractionThis resulting mixture was extracted with ethyl acetate
  3. washthis organic layer was washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationThe solvent was concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-1d0a9a6a73dc4aa487b5054ebe568ad1
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08829040B2

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