Hydrochloric Acid → HCID 25052188, Verbindung

HRID 881625

Reaktionsgleichung

Reaktionsgleichung von HRID 881625
C([O:3][C:4](=[O:40])[C:5]1[CH:10]=[CH:9][C:8]([N:11]2[C:19]3[C:14](=[CH:15][CH:16]=[C:17]([O:20][CH2:21][CH2:22][NH:23][C:24]([O:26][CH2:27][C:28]4[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=4)=[O:25])[CH:18]=3)[C:13]([C:34]#[N:35])=[CH:12]2)=[CH:7][C:6]=1[O:36]COC)C.C(O)C.O.[OH-].[Li+].Cl>O.O1CCCC1>[CH2:27]([O:26][C:24]([NH:23][CH2:22][CH2:21][O:20][C:17]1[CH:18]=[C:19]2[C:14]([C:13]([C:34]#[N:35])=[CH:12][N:11]2[C:8]2[CH:9]=[CH:10][C:5]([C:4]([OH:40])=[O:3])=[C:6]([OH:36])[CH:7]=2)=[CH:15][CH:16]=1)=[O:25])[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1

Komponenten

7

Edukt 4

HCID 313Hydrochloric Acid2×HCID 702EthanolHCID 168937Lithium hydroxide, monohydrateHCID 584372394-[6-(2-Benzyloxycarbonylaminoethyloxy)-3-cyanoindol-1-yl]-2-methoxymethoxy-benzoic acid ethyl ester

Produkt 1

HCID 25052188HCID 25052188, VerbindungAusbeute 79,9 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of 4-[6-(2-benzyloxycarbonylaminoethyloxy)-3-cyanoindol-1-yl]-2-methoxymethoxybenzoic acid ethyl ester (0.14 g) in a mixed solvent of ethanol (2.5 mL), tetrahydrofuran (5 mL), and water (2.5 mL) was added lithium hydroxide mono hydrate (0.03 g), and this mixture was stirred at room temperature for 3 hours. To this reaction mixture was added 2 mol/L hydrochloric acid (0.75 mL), and this mixture was stirred at 50° C. for 5 hours. This reaction mixture was treated 1 mol/L hydrochloric acid (5 mL), and this mixture was concentrated under reduced pressure until this solvent volume became one-third. The precipitated solid was collected by filtration, and washed with water, methanol and ether to give the title compound (0.097 g)

Aufarbeitung

  1. stirringthis mixture was stirred at 50° C. for 5 hours
  2. concentrationthis mixture was concentrated under reduced pressure until this solvent volume
  3. filtrationThe precipitated solid was collected by filtration
  4. washwashed with water, methanol and ether

Quellen und Nachweise

ORD-Eintrag
ord-ac3adb6d05124831924c73e4c4012838
Quelldatensatz
uspto-grants-2015_03
Patentnummer
US08993616B2

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