4-Fluorobenzylamine → HCID 178429626, Verbindung

HRID 23630

Reaktionsgleichung

Reaktionsgleichung von HRID 23630
[OH:1][C:2]1[C:7]([C:8]([O:10]CC)=O)=[CH:6][N:5]=[C:4]2[C:13]([CH3:18])=[C:14]([CH2:16][OH:17])[S:15][C:3]=12.[F:19][C:20]1[CH:27]=[CH:26][C:23]([CH2:24][NH2:25])=[CH:22][CH:21]=1>Cl>[F:19][C:20]1[CH:27]=[CH:26][C:23]([CH2:24][NH:25][C:8]([C:7]2[C:2]([OH:1])=[C:3]3[S:15][C:14]([CH2:16][OH:17])=[C:13]([CH3:18])[C:4]3=[N:5][CH:6]=2)=[O:10])=[CH:22][CH:21]=1

Komponenten

4

Edukt 2

HCID 673264-FluorobenzylamineHCID 178469552HCID 178469552, Verbindung

Produkt 1

HCID 178429626HCID 178429626, VerbindungAusbeute 85,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

A suspension of 140 mg (0.52 mmol) ethyl 7-hydroxy-2-(hydroxymethyl)-3-methylthieno[3,2-b]pyridine-6-carboxylate in 1.28 mL (11.2 mmol) 4-fluorobenzylamine was heated to 80° C. for 24 hours. The mixture was then cooled to room temperature and added to 10 mL of 1N HCl and then cooled in the refrigerator for three hours. The resulting mixture was then filtered and the obtained solid was washed with 1N HCl several times (50 mL total volume) and dried in a vacuum oven at 60° C. over night to provide 154 mg of the title compound as a tan solid.

Aufarbeitung

  1. temperatureThe mixture was then cooled to room temperature
  2. temperaturecooled in the refrigerator for three hours
  3. filtrationThe resulting mixture was then filtered
  4. washthe obtained solid was washed with 1N HCl several times (50 mL total volume)
  5. customdried in a vacuum oven at 60° C. over night

Quellen und Nachweise

ORD-Eintrag
ord-bc944c46c3124ec2806eac8d44ed2373
Quelldatensatz
uspto-grants-2005_02
Patentnummer
US06852731B2

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