反应详情

A solution of 1-ethylcyclopentyl methacrylate (ECPMA, M1; 20 mmol), 1-isopropyl-adamantanyl methacrylate (IAM, M2; 20 mmol), 2-oxo-tetrahydro-furan-3-yl methacrylate (α-GBLMA, M3; 30 mmol), 3-oxo-4,10-dioxa-tricyclo[5.2.1.02,6]dec-8(or 9)-yl methacrylate (ODOTMA, M4; 20 mmol), and 3-hydroxy-adamantanyl methacrylate (HAMA, M5; 10 mmol) dissolved in 30 g of tetrahydrofuran (THF) was degassed by bubbling with nitrogen and charged to a 500 ml flask equipped with a condenser, nitrogen inlet and mechanical stirrer along with an additional 10 g of degassed THF. The solution is brought to reflux, and 6 g of dimethyl-2,2-azodiisobutyrate is dissolved in 5 g of THF and charged in to the flask. The polymerization mixture is then stirred for about 4 hours at reflux, after which time the reaction is diluted with 5 g of THF and the polymerization mixture cooled to room temperature. The polymer is precipitated by addition to 1.0 L of isopropanol, the solid collected by filtration, re-precipitated by dissolving in 50 g THF and dropwise addition to another 1.0 L isopropanol, and the precipitated polymer collected and dried under vacuum at 45° C. for 48 h. to yield photoresist polymer poly(IAM/ECPMA/α-GBLMA/ODOTMA/HAMA) (20:20:30:20:10 ratio, respectively). Mw=8,000.

1. customwas degassed
2. customby bubbling with nitrogen
3. additioncharged to a 500 ml flask
4. customequipped with a condenser, nitrogen inlet and mechanical stirrer along with an additional 10 g of degassed THF
5. temperatureto reflux
6. dissolution6 g of dimethyl-2,2-azodiisobutyrate is dissolved in 5 g of THF
7. additioncharged in to the flask
8. temperatureat reflux
9. additionafter which time the reaction is diluted with 5 g of THF
10. customThe polymer is precipitated by addition to 1.0 L of isopropanol
11. filtrationthe solid collected by filtration
12. customre-precipitated
13. dissolutionby dissolving in 50 g THF
14. additiondropwise addition to another 1.0 L isopropanol
15. customthe precipitated polymer collected
16. customdried under vacuum at 45° C. for 48 h.