Reacción #11280

Ecuación de reacción

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

Disolventes

1,2-dichloroethane

heptane

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.DISSOLUTIONhad dissolved
2. 2
   TemperaturaOn cooling
3. 3
   FiltraciónThe insolubles were filtered off
4. 4
   Otrothe filtrate evaporated
5. 5
   Otroto give an oil
6. 6
   Filtraciónthe precipitated solid filtered off
7. 7
   SecadoThe remaining solution was dried (MgSO4)
8. 8
   Concentraciónconcentrated

Procedimiento

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.

Fuente