Reaktion #11280

Reaktionsgleichung

2,5-Dichlorobenzohydrazide

triethylamine

9,9-dioctyl-9H-fluorene-2-carbonyl chloride

→

desired intermediate

2,5-Dichloro-N′-[(9,9-dioctyl-9H-fluoren-2-yl)carbonyl]benzohydrazide

Lösungsmittel

1,2-dichloroethane

heptane

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.DISSOLUTIONhad dissolved
2. 2
   TemperaturOn cooling
3. 3
   FiltrationThe insolubles were filtered off
4. 4
   Sonstigethe filtrate evaporated
5. 5
   Sonstigeto give an oil
6. 6
   Filtrationthe precipitated solid filtered off
7. 7
   TrocknenThe remaining solution was dried (MgSO4)
8. 8
   Einengenconcentrated

Vorschrift

2,5-Dichlorobenzohydrazide (one equivalent) and triethylamine (one equivalent) were warmed in 500 mL of 1,2-dichloroethane until the solid material had dissolved. On cooling, 9,9-dioctyl-9H-fluorene-2-carbonyl chloride (one equivalent) was added and the mixture stirred at RT for two days. The insolubles were filtered off and the filtrate evaporated to give an oil. This was taken up in heptane and the precipitated solid filtered off. The remaining solution was dried (MgSO4) and concentrated to give the desired intermediate.

Quelle