Methanol → p-Tert-butoxystyrene p-methylstyrene

HRID 430907

반응식

HRID 430907 반응식
N(C(C)(CC)C([O-])=O)=NC(C)(CC)C([O-])=O.[C:17]([O:21][C:22]1[CH:29]=[CH:28][C:25]([CH:26]=[CH2:27])=[CH:24][CH:23]=1)([CH3:20])([CH3:19])[CH3:18].[CH3:30][C:31]1[CH:38]=[CH:37][C:34]([CH:35]=[CH2:36])=[CH:33][CH:32]=1.CO>O1CCOCC1>[C:17]([O:21][C:22]1[CH:23]=[CH:24][C:25]([CH:26]=[CH2:27])=[CH:28][CH:29]=1)([CH3:20])([CH3:18])[CH3:19].[CH3:30][C:31]1[CH:38]=[CH:37][C:34]([CH:35]=[CH2:36])=[CH:33][CH:32]=1

참가 물질

6

반응물 4

HCID 887MethanolHCID 121611-Ethenyl-4-methylbenzeneHCID 5775311-(Tert-butoxy)-4-ethenylbenzeneHCID 219175032,2'-Azobis(methyl 2-methylpropanate)

생성물 1

HCID 67612459p-Tert-butoxystyrene p-methylstyrene

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

2,2′-Azobis(methyl 2-methylpropionate) was added to a mixture of 100 g (0.567 mole) of p-tert-butoxystyrene and 3.54 g (0.03 mole) of p-methylstyrene in 1,4-dioxane, followed by conducting a polymerization reaction at 80° C. for 6 hours under nitrogen gas streams. After cooling, the reaction solution was poured into 5000 ml of aqueous methanol solution to precipitate out. The precipitated polymer was filtered, washed with methanol and dried under reduced pressure to give 92.3 g of poly(p-tert-butoxystyrene/p-methylstyrene) as white powders. A ratio of p-tert-butoxystyrene unit and p-methylstyrene unit was about 95:5 by 1HNMR. Mw was about 20000 and Mw/Mn was 1.90 by GPC measurement using polystyrene as standard.

후처리

  1. customa polymerization reaction at 80° C. for 6 hours under nitrogen gas streams
  2. temperatureAfter cooling
  3. customto precipitate out
  4. filtrationThe precipitated polymer was filtered
  5. washwashed with methanol
  6. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-ecdc3ce1f081466aaa85836965880355
출처 데이터셋
uspto-grants-2003_12
특허 번호
US06656660B1

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