反应 #1483142

反应方程式

1-ethylcyclopentyl methacrylate

1-isopropyl-adamantanyl methacrylate

2-oxo-tetrahydro-furan-3-yl methacrylate

3-hydroxy-adamantanyl methacrylate

→

IAM ECPMA

HAMA

溶剂

tetrahydrofuran

反应条件

后处理

1. 1
   其他is degassed
2. 2
   其他by bubbling with nitrogen
3. 3
   workup.ADDITIONcharged to a 500 ml flask
4. 4
   其他equipped with a condenser, nitrogen inlet and mechanical stirrer along with an additional 10 g of degassed THF
5. 5
   温度to reflux
6. 6
   workup.DISSOLUTION6 g of dimethyl-2,2-azodiisobutyrate is dissolved in 5 g of THF
7. 7
   workup.ADDITIONcharged in to the flask
8. 8
   温度at reflux
9. 9
   workup.ADDITIONafter which time the reaction is diluted with 5 g of THF
10. 10
    其他The polymer is precipitated by addition to 1.0 L of isopropanol
11. 11
    过滤collected by filtration
12. 12
    其他re-precipitated
13. 13
    workup.DISSOLUTIONby dissolving in 50 g THF
14. 14
    workup.ADDITIONaddition to another 1.0 L isopropanol
15. 15
    其他collected
16. 16
    其他dried under vacuum at 45° C. for 48 h.

实验过程

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) is 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, collected by filtration, re-precipitated by dissolving in 50 g THF and addition to another 1.0 L isopropanol, and collected and dried under vacuum at 45° C. for 48 h. to yield photoresist polymer poly(IAM/ECPMA/α-GBLMA/ODOTMA/HAMA). Mw=8,000.

来源