Styrene → Isobutylene styrene

HRID 526312노트

반응식

HRID 526312 반응식
[CH3:1][CH:2]1[CH2:7]CCC[CH2:3]1.[C:8](Cl)([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)(C)[CH3:9].N1C=CC=CC=1C.CC(=C)C.C=CC1C=CC=CC=1>[Ti](Cl)(Cl)(Cl)Cl.CO.C(Cl)CCC>[CH2:9]=[CH:8][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[CH3:3][C:2](=[CH2:1])[CH3:7]

참가 물질

9

반응물 5

HCID 7501StyreneHCID 7962MethylcyclohexaneHCID 79752-MethylpyridineHCID 8255IsobutyleneHCID 70281(1-Chloro-1-methylethyl)benzene

생성물 1

HCID 44154101Isobutylene styrene

시약·촉매·용매 3

HCID 24193Titanium Tetrachloride촉매HCID 887Methanol용매HCID 8005Butyl Chloride용매

반응 조건

온도
-70 °C

실험 절차

Into a 2 L reaction container having an agitator, 589 mL of methylcyclohexane (dried with molecular sieves), 613 ml of n-butyl chloride (dried with molecular sieves), and 0.550 g of cumyl chloride were added. The reaction container was cooled to −70° C., and then 0.35 mL of α-picoline (2-methylpyridine) and 179 mL of isobutylene were added. Further, 9.4 mL of titanium tetrachloride was added to start polymerization. They were reacted with each other for 2.0 hours while stirring the solution at −70° C. Next, 59 mL of styrene was added to the reaction container, and reaction was continued for another 60 minutes. Thereafter, a large amount of methanol was added to stop the reaction. After removing a solvent and the like from the reaction solution, the polymer was dissolved with toluene and rinsed twice. This toluene solution was added to a methanol mixture to precipitate a polymer. The polymer thus obtained was dried at 60° C. for 24 hours, thereby obtaining a styrene-isobutylene diblock copolymer.

후처리

  1. customInto a 2 L reaction container
  2. additionwere added
  3. custompolymerization
  4. customThey were reacted with each other for 2.0 hours
  5. customthe reaction
  6. customAfter removing a solvent
  7. dissolutionthe like from the reaction solution, the polymer was dissolved with toluene
  8. washrinsed twice
  9. additionThis toluene solution was added to a methanol mixture
  10. customto precipitate a polymer
  11. customThe polymer thus obtained
  12. customwas dried at 60° C. for 24 hours

출처 및 근거

ORD 기록
ord-33458a051763415d9db0f0a2940d31aa
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09346227B2

반응 노트

불러오는 중…