تفاعل #955970

معادلة التفاعل

(4-(3-ethylhept-1-yn-1-yl)-8-(3-ethylnon-1-yn-1-yl)benzo[1,2-b:4,5-b′]dithiophene-2,6-diyl)bis(triisopropylsilane)

→

solid

المردود 97.1%

(4,8-bis(3-ethylheptyl)benzo[1,2-b:4,5-b′]dithiophene-2,6-diyl)bis(triisopropylsilane)

المردود 97.1%

ظروف التفاعل

المعالجة

1. 1
   أخرىA dry 100 mL three-neck round bottom flask equipped with a condenser
2. 2
   أخرىwas flushed with N2
3. 3
   تجفيفdry support (0.70 g, 10%) and anhydrous 1,4-dioxane (30 mL, 0.11 M)
4. 4
   أخرىThe flask was evacuated
5. 5
   درجة الحرارةthe mixture was cooled to ambient temperature
6. 6
   ترشيحfiltered through Celite, and solvent
7. 7
   أخرىwas removed by rotary evaporation
8. 8
   workup.DISSOLUTIONThe solid was dissolved in chloroform
9. 9
   أخرىprecipitated into methanol

الإجراء التجريبي

A dry 100 mL three-neck round bottom flask equipped with a condenser was flushed with N2 and was charged with (4-(3-ethylhept-1-yn-1-yl)-8-(3-ethylnon-1-yn-1-yl)benzo[1,2-b:4,5-b′]dithiophene-2,6-diyl)bis(triisopropylsilane) (2.5 g, 3.3 mmol), Pd/C dry support (0.70 g, 10%) and anhydrous 1,4-dioxane (30 mL, 0.11 M). The flask was evacuated and backfilled with hydrogen. The reaction was kept under a hydrogen atmosphere and slowly heated to 95° C. Completion of hydrogenation was monitored by TLC. After hydrogenation was complete, the mixture was cooled to ambient temperature, filtered through Celite, and solvent was removed by rotary evaporation. The solid was dissolved in chloroform and precipitated into methanol to yield white solid (2.42 g, 97%).

المصدر