반응 #11280

반응 방정식

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

용매

1,2-dichloroethane

heptane

반응 조건

후처리

1. 1
   workup.DISSOLUTIONhad dissolved
2. 2
   온도On cooling
3. 3
   여과The insolubles were filtered off
4. 4
   기타the filtrate evaporated
5. 5
   기타to give an oil
6. 6
   여과the precipitated solid filtered off
7. 7
   건조The remaining solution was dried (MgSO4)
8. 8
   농축concentrated

실험 절차

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.

출처