1-Hexene → Decyl Norbornene Phenylethyl Norbornene

HRID 1161626노트

반응식

HRID 1161626 반응식
[CH2:1]([C:11]12[CH2:17][CH:14]([CH2:15][CH2:16]1)[CH:13]=[CH:12]2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10].C=CCCCC>ClCCl.C1COCC1.C1(C)C=CC=CC=1>[CH2:1]([C:11]12[CH2:17][CH:14]([CH2:15][CH2:16]1)[CH:13]=[CH:12]2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10].[C:3]1([CH2:2][CH2:1][C:11]23[CH2:17][CH:14]([CH2:15][CH2:16]2)[CH:13]=[CH:12]3)[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1

참가 물질

6

반응물 2

HCID 115971-HexeneHCID 21922320Decyl Norbornene2회

생성물 1

HCID 86613230Decyl Norbornene Phenylethyl Norbornene

시약·촉매·용매 3

HCID 1140Toluene용매2회HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매

반응 조건

온도
80 °C

실험 절차

Decyl Norbornene (DeNB, CAS 22094-85-5) (6.84 g, 0.029 mol), PENB (23.16 g, 0.117 mol), 1-hexene (12.26 g, 0.146 mol) and toluene (170.0 g) were combined in a 500 mL serum bottle and heated to 80° C. in an oil bath to form a solution. To this solution were injected Pd1446 (0.0084 g, 5.84E-06 mol) and DANFABA (0.019 g, 2.33E-5 mol), each in the form of a concentrated solution in dichloromethane. After addition, the resulting mixture was maintained at 80° C. for 50 minutes. The copolymer was precipitated by adding methanol drop wise into the vigorously stirred reaction mixture. The precipitated copolymer was collected by filtration and dried in an oven at 60° C. under vacuum. After drying, 19.74 g was obtained (66%). The molecular weight of the copolymer was determined by GPC in THF solvent (polystyrene standard) to be Mw=78,000 and Mn=36,000. The composition of the copolymer was determined by 1H-NMR to be (19/81) DeNB/PENB copolymer. The refractive indices of this polymer were measured by prism coupling method and determined to be 1.5640 in TE mode and 1.5622 in TM mode at a wavelength of 633 nm The dried copolymer was dissolved in sufficient toluene to result in a 30 wt % copolymer solution.

후처리

  1. customto form a solution
  2. additionAfter addition
  3. temperaturethe resulting mixture was maintained at 80° C. for 50 minutes
  4. customThe copolymer was precipitated
  5. additionby adding methanol
  6. customdrop wise into the vigorously stirred reaction mixture
  7. filtrationThe precipitated copolymer was collected by filtration
  8. customdried in an oven at 60° C. under vacuum
  9. customAfter drying
  10. custom19.74 g was obtained (66%)
  11. customto result in a 30 wt % copolymer solution

출처 및 근거

ORD 기록
ord-345ea9c45a63402a8cec95bc413c81c7
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07820356B2

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