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Sodium Hydroxide → HCID 21995280, Verbindung

HRID 1977684
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1977684
C([O:3][C:4]([CH2:6][C:7]1[CH:12]=[CH:11][C:10]([NH:13][C:14]2[CH:19]=[CH:18][N:17]=[C:16]([NH:20][C:21]3[CH:26]=[C:25]([O:27][CH3:28])[C:24]([O:29][CH3:30])=[C:23]([O:31][CH3:32])[CH:22]=3)[N:15]=2)=[CH:9][CH:8]=1)=[O:5])C.[OH-].[Na+]>C(O)C>[C:4]([CH2:6][C:7]1[CH:8]=[CH:9][C:10]([NH:13][C:14]2[CH:19]=[CH:18][N:17]=[C:16]([NH:20][C:21]3[CH:22]=[C:23]([O:31][CH3:32])[C:24]([O:29][CH3:30])=[C:25]([O:27][CH3:28])[CH:26]=3)[N:15]=2)=[CH:11][CH:12]=1)([OH:5])=[O:3]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 21995173HCID 21995173, Verbindung

Produkt 1

HCID 21995280HCID 21995280, VerbindungAusbeute 38 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel2×

Versuchsvorschrift

The compound of Example 103 (250 mg, 0.57 mmol) in a solution of ethanol (10 ml) containing 6N aqueous NaOH (2.0 ml) was heated a reflux for 2 h. On cooling the ethanol was removed under reduced pressure and the basic solution brought to pH 5 with 2M hydrochloric acid. The resulting solution was concentrated under reduced pressure, and the residue taken up in hot ethanol (20 ml). This solution was filtered and the filtrate evaporated under reduced pressure to give a residue which was crystalised from ethanol to give the title compound (89 mg) as a white solid m.p. 144-150°. MS m/z 411 (M+H)+.

Aufarbeitung

  1. temperaturewas heated
  2. temperaturea reflux for 2 h
  3. customwas removed under reduced pressure
  4. concentrationThe resulting solution was concentrated under reduced pressure
  5. filtrationThis solution was filtered
  6. customthe filtrate evaporated under reduced pressure
  7. customto give a residue which
  8. customwas crystalised from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-a23b4981961e4b07982ff40c14e2d63a
Quelldatensatz
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06235746B1

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