Ethyl 2-formylbutanoate → HCID 178457579, Verbindung

HRID 1253164

Reaktionsgleichung

Reaktionsgleichung von HRID 1253164
Cl.[CH2:2]([N:5]=[C:6]([NH2:21])[NH:7][C:8]1[CH:13]=[CH:12][N:11]=[C:10]([CH2:14][CH2:15][CH2:16][CH2:17][C:18]([NH2:20])=[NH:19])[N:9]=1)[CH2:3][CH3:4].[Na].[CH:23]([CH:25]([CH2:31][CH3:32])[C:26](OCC)=O)=[O:24]>CO>[CH2:2]([N:5]=[C:6]([NH2:21])[NH:7][C:8]1[CH:13]=[CH:12][N:11]=[C:10]([CH2:14][CH2:15][CH2:16][CH2:17][C:18]2[N:20]=[C:23]([OH:24])[C:25]([CH2:31][CH3:32])=[CH:26][N:19]=2)[N:9]=1)[CH2:3][CH3:4]

Komponenten

5

Edukt 3

HCID 289299Ethyl 2-formylbutanoateHCID 5360545SodiumHCID 201371495-(4-[2-Propylguanidino]pyrimid-2-yl)valeramidine hydrochloride

Produkt 1

HCID 178457579HCID 178457579, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A mixture of 5-(4-[2-propylguanidino]pyrimid-2-yl)valeramidine hydrochloride (0.4 g.) and the sodium salt of ethyl 2-formylbutyrate (1.5 g.) in MeOH (5 ml.) was heated under reflux for 4 hours. The solvent was evaporated in vacuo and the residue was partitioned between water (pH 7) and EtOAc. The EtOAc layer was separated, dried (MgSO4) and evaporated in vacuo to give 2-[4-(4-(2-propylguanidino]pyrimid-2-yl)butyl]-5-ethyl-4-hydroxypyrimidine as an oil (0.13 g.) which was characterised by conversion to the bis hydrogen maleate salt (0.11 g.), m.p. 140°-142°.

Aufarbeitung

  1. temperatureunder reflux for 4 hours
  2. customThe solvent was evaporated in vacuo
  3. customthe residue was partitioned between water (pH 7) and EtOAc
  4. customThe EtOAc layer was separated
  5. dry with materialdried (MgSO4)
  6. customevaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-6d6b062b552241ad9e238f1746723804
Quelldatensatz
uspto-grants-1988_05
Patentnummer
US04748165

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