gamma-Butyrolactone methacrylate → 3-Hydroxy-1-methacryloyloxyadamantane

HRID 1471323

반응식

HRID 1471323 반응식
[C:1]([O:6][CH:7]1[CH:14]2[CH2:15][CH:10]3[CH2:11][CH:12]([CH2:16][C:8]1([CH:17]([CH3:19])[CH3:18])[CH2:9]3)[CH2:13]2)(=[O:5])[C:2]([CH3:4])=[CH2:3].[C:20]([O:25][C:26]1([CH2:31][CH3:32])[CH2:30][CH2:29][CH2:28][CH2:27]1)(=[O:24])[C:21]([CH3:23])=[CH2:22].C(OC1CCOC1=O)(=O)C(C)=C.[C:45]([O:50][C:51]12[CH2:60][CH:55]3[CH2:56][CH:57]([CH2:59][C:53]([OH:61])([CH2:54]3)[CH2:52]1)[CH2:58]2)(=[O:49])[C:46]([CH3:48])=[CH2:47]>O1CCCC1>[C:1]([O:6][CH:7]1[CH:14]2[CH2:13][CH:12]3[CH2:11][CH:10]([CH2:9][C:8]1([CH:17]([CH3:19])[CH3:18])[CH2:16]3)[CH2:15]2)(=[O:5])[C:2]([CH3:4])=[CH2:3].[C:20]([O:25][C:26]1([CH2:31][CH3:32])[CH2:30][CH2:29][CH2:28][CH2:27]1)(=[O:24])[C:21]([CH3:23])=[CH2:22].[C:45]([O:50][C:51]12[CH2:58][CH:57]3[CH2:56][CH:55]([CH2:54][C:53]([OH:61])([CH2:59]3)[CH2:52]1)[CH2:60]2)(=[O:49])[C:46]([CH3:48])=[CH2:47]

참가 물질

7

반응물 4

HCID 11206014gamma-Butyrolactone methacrylateHCID 118565233-Hydroxy-1-methacryloyloxyadamantaneHCID 180005792-Propenoic acid, 2-methyl-, 1-ethylcyclopentyl ester (9CI, ACI)HCID 668625631-Isopropyl-adamantanyl methacrylate

생성물 2

HCID 118565233-Hydroxy-1-methacryloyloxyadamantaneHCID 131731389Iam ecpma

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A photoresist polymer for use in the lithographic evaluations (below) is prepared according to the following procedure. A solution of 1-isopropyl-adamantanyl methacrylate (IAM) (20 mmol), 1-ethylcyclopentyl methacrylate (ECPMA)(20 mmol), 2-oxo-tetrahydro-furan-3-yl methacrylate (α-GBLMA) (30 mmol), 3-oxo-4,10-dioxa-tricyclo[5.2.1.02,6]dec-8(or 9)-yl methacrylate (ODOTMA) (20 mmol), and 3-hydroxy-adamantanyl methacrylate (HAMA) (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 5 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=9,000.

후처리

  1. customA photoresist polymer for use in the lithographic evaluations (below) is prepared
  2. customis degassed
  3. customby bubbling with nitrogen
  4. additioncharged to a 500 ml flask
  5. customequipped with a condenser, nitrogen inlet and mechanical stirrer along with an additional 10 g of degassed THF
  6. temperatureto reflux
  7. dissolution5 g of dimethyl-2,2-azodiisobutyrate is dissolved in 5 g of THF
  8. additioncharged in to the flask
  9. temperatureat reflux
  10. additionafter which time the reaction is diluted with 5 g of THF
  11. customThe polymer is precipitated by addition to 1.0 L of isopropanol
  12. filtrationcollected by filtration
  13. customre-precipitated
  14. dissolutionby dissolving in 50 g THF
  15. additionaddition to another 1.0 L isopropanol
  16. customcollected
  17. customdried under vacuum at 45° C. for 48 h.

출처 및 근거

ORD 기록
ord-7903ced116f34756870b0c91cf84a2c8
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09012128B2

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