反応 #11280

反応方程式

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

溶媒

1,2-dichloroethane

heptane

反応条件

後処理

1. 1
   workup.DISSOLUTIONhad dissolved
2. 2
   温度On cooling
3. 3
   ろ過The insolubles were filtered off
4. 4
   その他the filtrate evaporated
5. 5
   その他to give an oil
6. 6
   ろ過the precipitated solid filtered off
7. 7
   乾燥The remaining solution was dried (MgSO4)
8. 8
   濃縮concentrated

実験手順

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.

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