Trimethyl orthoacetate → HCID 14232984, Verbindung

HRID 985955Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 985955
[NH2:1][C:2]1[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:3]=1[C:4]([NH:6][CH2:7][CH2:8][CH2:9][N:10]1[CH:14]=[CH:13][N:12]=[CH:11]1)=[O:5].[C:20](OC)(OC)(OC)[CH3:21]>C(O)C>[Cl:19][C:16]1[CH:15]=[C:3]2[C:2](=[CH:18][CH:17]=1)[N:1]=[C:20]([CH3:21])[N:6]([CH2:7][CH2:8][CH2:9][N:10]1[CH:14]=[CH:13][N:12]=[CH:11]1)[C:4]2=[O:5]

Komponenten

4

Edukt 2

HCID 15050Trimethyl orthoacetateHCID 135889602-Amino-5-chloro-N-[3-(1H-imidazol-1-yl)propyl]benzamide

Produkt 1

HCID 14232984HCID 14232984, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 2.79 g of 2-amino-5-chloro-N-[3-(1H-imidazol-1-yl)propyl]benzamide, 5 ml of trimethyl orthoacetate and 10 ml of ethyl alcohol was heated at reflux for 24 hours. The resulting solution was concentrated and the residue was triturated with ether and gave a solid. The ether was decanted and the solid was dissolved in ethyl acetate and allowed to stand. The precipitate was collected and gave 650 mg of the desired product as tan crystals, mp 190°-192° C.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureat reflux for 24 hours
  3. concentrationThe resulting solution was concentrated
  4. customthe residue was triturated with ether
  5. customgave a solid
  6. customThe ether was decanted
  7. dissolutionthe solid was dissolved in ethyl acetate
  8. customThe precipitate was collected

Quellen und Nachweise

ORD-Eintrag
ord-8fa131882a6140489464c49bb5ce5904
Quelldatensatz
uspto-grants-1987_12
Patentnummer
US04710502

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