Reaktion #1788320

Reaktionsgleichung

1,5-bis[p-(trifluoromethoxy)phenyl]-1,4-pentadien-3-one

4,5,6,7-tetrahydro-1H-1,3-diazepine-2-ylhydrazine hydroiodide

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title product

Ausbeute 75.0%

1,5-Bis[p-(trifluoromethoxy)phenyl]-1,4-pentadien-3-one-4,5,6,7-tetrahydro-1H-1,3-diazepin-2-ylhydrazone

Ausbeute 75.0%

Lösungsmittel

isopropyl alcohol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturis heated
2. 2
   Temperaturat reflux for 2 to 3 hours
3. 3
   Sonstigethe precipitated material is isolated by filtration
4. 4
   Waschenwashed with ether
5. 5
   workup.ADDITIONThe isolated material is mixed with ether and saturated sodium carbonate solution
6. 6
   SonstigeThe ether layer is then separated
7. 7
   Sonstigedried
8. 8
   Einengenconcentrated

Vorschrift

A mixture of 1,5-bis[p-(trifluoromethoxy)phenyl]-1,4-pentadien-3-one (4.0 g; 0.01 mole), 4,5,6,7-tetrahydro-1H-1,3-diazepine-2-ylhydrazine hydroiodide (2.6 g; 0.01 mole) and isopropyl alcohol (25 ml) is heated at reflux for 2 to 3 hours. The reaction mixture is then cooled to -15° C., and the precipitated material is isolated by filtration and washed with ether. The isolated material is mixed with ether and saturated sodium carbonate solution and the mixture stirred for about 15 minutes. The ether layer is then separated, dried, and concentrated to afford 3.8 g (75%) of title product, a bright yellow solid, m.p. 184.5°-185.5° C.

Quelle