反応 #714995

反応方程式

Methyl methacrylate

dimethylketene methyl trimethylsilyl acetal

tetrabutylammonium m-chlorobenzoate

dimethylaminoethyl methacrylate

→

propylene glycol monomethyl ether acetate

溶媒

acetonitrile

methanol

Tetrahydrofuran

反応条件

後処理

1. 1
   その他A 500 mL four-necked round-bottom separable flask was equipped with a condenser tube, a dropping funnel, a nitrogen inlet, a stirrer
2. 2
   workup.ADDITIONwere poured into the flask through the dropping funnel
3. 3
   その他was injected with a syringe
4. 4
   温度While cooling the separable flask
5. 5
   その他was kept below 40° C
6. 6
   workup.ADDITIONwas added
7. 7
   その他to terminate
8. 8
   その他the reaction
9. 9
   その他The thus-obtained copolymer THF solution was reprecipitated in hexane
10. 10
    ろ過filtrated
11. 11
    その他dried in vacuum
12. 12
    その他purified
13. 13
    その他thus obtaining a polymer

実験手順

A 500 mL four-necked round-bottom separable flask was equipped with a condenser tube, a dropping funnel, a nitrogen inlet, a stirrer and a thermometer. Tetrahydrofuran (THF) of 250 parts by weight and dimethylketene methyl trimethylsilyl acetal of 2.32 parts by weight, which is an initiator, were poured into the flask through the dropping funnel, followed by sufficient nitrogen substitution. Then, 0.2 part by weight of 1 mol/L acetonitrile solution of tetrabutylammonium m-chlorobenzoate, which is a catalyst, was injected with a syringe. Methyl methacrylate (hereinafter may be referred to as MMA) of 93.3 parts by weight was added dropwise with the dropping funnel for 60 minutes. While cooling the separable flask, the temperature was kept below 40° C. One hour later, dimethylaminoethyl methacrylate (hereinafter may be referred to as DMMA) of 40.0 parts by weight was added dropwise for 20 minutes. After one hour reaction, methanol of 0.5 parts by mass was added to terminate the reaction. The thus-obtained copolymer THF solution was reprecipitated in hexane, filtrated, dried in vacuum and then purified, thus obtaining a polymer. To the amine-containing polymer obtained in this manner of 60 parts by weight, propylene glycol monomethyl ether acetate (hereinafter may be referred to as PGMEA) of 40 parts by weight was added and uniformly mixed to obtain a polymer solution B1. For the polymer solution B1, GPC was measured with HLC-8220 equipped with an RI detector (manufactured by Tosoh Corporation), using THF as the developing solvent and a molecular weight standard polymer as the standard polystyrene, thus obtaining the molecular weight distribution and mass average molecular weight. The amine value was 115 mg KOH/g. The mass average molecular weight Mw was 9,900. The number average molecular weight Mn was 8,320. The molecular weight distribution Mw/Mn was 1.19 (MMA/DMMA mass ratio: 7/3).

出典