Reaktion #1706602

Reaktionsgleichung

(E)-7-methoxy-4-methyl-3,4,5,6-tetrahydro-2H-azepine

2-aminoterephthalic acid

→

desired product

Ausbeute 2.2%

8-methyl-12-oxo-6,7,8,9,10,12-hexahydroazepino[2,1-b]quinazoline-3-carboxylic acid

Ausbeute 2.2%

Lösungsmittel

water

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionextracted with ethyl acetate (2×60 mL)
2. 2
   WaschenThe combined organic layers were washed with brine
3. 3
   Trocknendried over anhydrous sodium sulfate
4. 4
   FiltrationAfter filtration and concentration
5. 5
   Sonstigethe crude product was purified by silica gel chromatography

Vorschrift

A solution of (E)-7-methoxy-4-methyl-3,4,5,6-tetrahydro-2H-azepine (1.1 g) and 2-aminoterephthalic acid (1.4 g, 7.7 mmol) in DMF (30 mL) was stirred at 100° C. for 4 h. After it was cooled to room temperature, the reaction was diluted with water (80 mL) and extracted with ethyl acetate (2×60 mL). The combined organic layers were washed with brine and dried over anhydrous sodium sulfate. After filtration and concentration, the crude product was purified by silica gel chromatography to give 47 mg of desired product.

Quelle