反応 #823762

反応方程式

Ethylaluminum sesquichloride

Norbornene

methyl methacrylate

AIBN

HCl MeOH

ethylaluminum sesquichloride

→

norbornene methyl methacrylate

溶媒

toluene

toluene

toluene

反応条件

後処理

1. 1
   workup.WAITthe reaction was performed at 65° C. for 12 hours
2. 2
   その他during the reaction
3. 3
   その他to precipitate a white polymer, which
4. 4
   ろ過was filtered through a glass
5. 5
   ろ過filter
6. 6
   その他dried in a vacuum oven at 70° C. for 12 hours

実験手順

Norbornene (8.8 g, 93 mmol), methyl methacrylate (5 mL, 47 mmol), and AIBN (0.23 g, 1.40 mmol) were charged into a 250 mL Schlenk flask and dissolved in 30 mL of toluene. Ethylaluminum sesquichloride (12.7 g, 51.4 mmol) was charged into a 100 mL flask and dissolved in 20 mL of toluene. The toluene solution of ethylaluminum sesquichloride was slowly dropped to the 250 mL Schlenk flask at −70° C. The reaction temperature was raised to room temperature while stirring the mixture for 2 hours, and then the reaction was performed at 65° C. for 12 hours. The reaction solution turned to light green in color during the reaction. After the reaction was completed, the reaction solution was slowly dropped to 3000 cc of 5% v/v HCl—MeOH to precipitate a white polymer, which was filtered through a glass filter and dried in a vacuum oven at 70° C. for 12 hours to obtain a norbornene-methyl methacrylate copolymer (0.3 g: 3.0% by weight based on the total weight of used monomers). The copolymer had a Tg of 167° C., a molecular weight (Mw) of 10,700, and Mw/Mn of 3.4.

出典