تفاعل #11280

معادلة التفاعل

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

المذيبات

1,2-dichloroethane

heptane

ظروف التفاعل

المعالجة

1. 1
   workup.DISSOLUTIONhad dissolved
2. 2
   درجة الحرارةOn cooling
3. 3
   ترشيحThe insolubles were filtered off
4. 4
   أخرىthe filtrate evaporated
5. 5
   أخرىto give an oil
6. 6
   ترشيحthe precipitated solid filtered off
7. 7
   تجفيفThe remaining solution was dried (MgSO4)
8. 8
   تركيزconcentrated

الإجراء التجريبي

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.

المصدر