Reaktion #172450

Reaktionsgleichung

5-[2-(8-methoxy-2,3,6,7-tetrahydro-1H,5H-benzo[ij]quinolizine-9-yl)vinyl]thiophene-2-carboaldehyde

2-(3-cyano-4,5,5-trimethyl-2(5H)-furanylidene)propanedinitrile

ammonium acetate

→

black powdered crystal

Ausbeute 62.0%

2-[3-cyano-4-[2-[5-[2-(8-methoxy-2,3,6,7-tetrahydro-1H,5H-benzo[ij]quinolizine-9-yl)vinyl]thiophene-2-yl]vinyl]-5,5-dimethyl-2(5H)-furanylidene]propanedinitrile

Ausbeute 62.0%

Lösungsmittel

ethanol

tetrahydrofuran

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationThe crystal was filtrated
2. 2
   Waschenwashed with ethanol
3. 3
   SonstigeThe residue was purified by silica gel column chromatography
4. 4
   Waschenwashed with ethanol

Vorschrift

In 5 ml of ethanol and 1.5 ml of tetrahydrofuran were dissolved 158 mg (0.47 mmol) of 5-[2-(8-methoxy-2,3,6,7-tetrahydro-1H,5H-benzo[ij]quinolizine-9-yl)vinyl]thiophene-2-carboaldehyde and 102 mg (0.51 mmol) of 2-(3-cyano-4,5,5-trimethyl-2(5H)-furanylidene)propanedinitrile. To this mixture was added 36 mg of ammonium acetate, and the mixture was stirred at room temperature for 42 hours. The crystal was filtrated and washed with ethanol. The residue was purified by silica gel column chromatography and washed with ethanol to give 150 mg of a black powdered crystal (yield: 62.0%; mp: 201-204° C.).

Quelle