Ring-opening polymerizations initiated by anionic reagents

Ring-opening polymerizations initiated by anionic reagents 

Caution Carry out all procedures in a well-ventilated fume-hood, wear appropriate disposable gloves, a lab-coat, and safety glasses. All vacuum-line work should be performed while standing behind a protective Perspex screen. Never use flat-bottomed flasks with rotary evaporators. 

Hexaoxa-1,10-diazabicyclo 8,8,8 hexacosane irritating to eyes, skin, and respiratory system 

Preparation. All glassware must be dried in the oven prior to use. 1,1-Diphenylethene is distilled under reduced pressure (b.p. 113 at 2 mmHg) from a small amount of potassium into a two-necked round-bottomed flask fitted with a septum and connected to the distillation apparatus via a Youngs tap such that the collecting flask can be filled with argon and removed from the distillation apparatus. Carbazole is purified by recrystallization from toluene, followed by methanol, and then sublimed in vacuum. 4,7,13,16,21,24-Hexaoxa-1,10-diazabicyclo[8,8,8] hexacosane (Kryptofix 222) is dried by placing the required amount in a round-bottomed flask and heating at 60°C for 24 h. 

Potassium (0.5 g, 13 mmol) is placed in a two-necked round-bottomed flask (50 ml) fitted with a rubber septum and connected to the dual manifold by a gas-inlet tube. A potassium mirror is created by evacuating the flask and heating the potassium (caution ). The flask is then placed under an atmosphere of argon and dry THF (10 mL, see Table 2.2) is added by syringe and the mixture is cooled in a dry ice/acetone mixture ( 78°C). 1,1-Diphenylethene (0.6 mL, 

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