Methanol → p-Tert-butoxystyrene p-methylstyrene

HRID 1600493Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1600493
[C:1]([O:5][C:6]1[CH:13]=[CH:12][C:9]([CH:10]=[CH2:11])=[CH:8][CH:7]=1)([CH3:4])([CH3:3])[CH3:2].[CH3:14][C:15]1[CH:22]=[CH:21][C:18]([CH:19]=[CH2:20])=[CH:17][CH:16]=1.N(C(C)(CC)C([O-])=O)=NC(C)(CC)C([O-])=O.CO>O1CCOCC1>[C:1]([O:5][C:6]1[CH:7]=[CH:8][C:9]([CH:10]=[CH2:11])=[CH:12][CH:13]=1)([CH3:4])([CH3:2])[CH3:3].[CH3:14][C:15]1[CH:22]=[CH:21][C:18]([CH:19]=[CH2:20])=[CH:17][CH:16]=1

Komponenten

6

Edukt 4

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

Produkt 1

HCID 67612459p-Tert-butoxystyrene p-methylstyrene

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

To a solution of 100 g (0.567 mol) of p-tert-butoxystyrene and 3.54 g (0.03 mol) of p-methylstyrene in 300 ml of 1,4-dioxane was added a catalytic amount of 2,2'-azobis(methyl 2-methylpropionate) to carry out reaction in a nitrogen stream at 80° for 6 hours. The reaction solution was cooled and poured into 5,000 ml of a methanol solution to cause crystallization. Precipitated crystals were filtered out, washed with methanol and dried in vacuo to give 92.3 g of poly-(p-tert-butoxystyrene/p-methylstyrene)as white powder. The polymer was found to have p-tert-butoxystyrene unit and p-methylstyrene unit in a molar ratio of ca. 95:5 based on 1H NMR. The weight-average molecular weight (Mw) was determined to be about 20,000 by GPC with polystyrene calibration.

Aufarbeitung

  1. customreaction in a nitrogen stream at 80° for 6 hours
  2. temperatureThe reaction solution was cooled
  3. customcrystallization
  4. customPrecipitated crystals
  5. filtrationwere filtered out
  6. washwashed with methanol
  7. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-bf44012fb98d40d38f3334174e1d2dba
Quelldatensatz
uspto-grants-1999_11
Patentnummer
US05976759

Notizen zur Reaktion

Wird geladen…