反応 #2507810

反応方程式

diisopropyl azodicarboxylate

Pentacene maleimide

Pentacene Maleimide

triphenyl phosphine

11-bromo-1-undecanol

→

5d

N-(11-bromoundecyl) maleimide pentacene

11-bromoundecylmaleimide pentacene

溶媒

THF

tetrahydrofuran

反応条件

後処理

1. 1
   workup.ADDITIONAfter completion of the addition
2. 2
   その他The solvent is evaporated under reduced pressure
3. 3
   ろ過the precipitate is filtered
4. 4
   洗浄washed with 1:1 ether-hexane
5. 5
   その他dried
6. 6
   その他Crystallization from benzene

実験手順

Pentacene-maleimide adduct (5c) (375 mg, 1 mmole) are added to a solution of triphenyl phosphine (393 mg, 1.5 mmole) and 11-bromo-1-undecanol (375 mg, 1.5 mmole) in 40 mL of anhydrous tetrahydrofuran. To this mixture a solution of diisopropyl azodicarboxylate (300 mg, 1.5 mmole) in 10 mL of anhydrous THF is added dropwise under a stream of nitrogen. After completion of the addition, the solution is stirred at room temperature for 18 hours. The solvent is evaporated under reduced pressure and the residue is titrated with diethyl ether and the precipitate is filtered, washed with 1:1 ether-hexane and dried. Crystallization from benzene affords the pure sample of 11-bromoundecylmaleimide-pentacene adduct 5d.

出典