반응 #955970

반응 방정식

(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

수율 97.1%

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

수율 97.1%

반응 조건

후처리

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

실험 절차

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%).

출처