Reaktion #65312

Reaktionsgleichung

m-cresol

2,6-bis(hydroxymethyl)-p-cresol

3-mercaptopropionic acid

p-toluene-sulfonic acid monohydrate

salicylaldehyde

→

m-cresol-salicylaldehyde

Lösungsmittel

acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeequipped with a paddle stirrer
2. 2
   Temperaturreflux condenser and a nitrogen inlet tube
3. 3
   TemperaturThe mixture was heated
4. 4
   Temperaturto reflux
5. 5
   Temperaturmaintained
6. 6
   Temperaturat reflux

Vorschrift

A mixture of 146.0 g m-cresol, 25.2 g 2,6-bis(hydroxymethyl)-p-cresol, 5.0 g 3-mercaptopropionic acid and 1.5 g p-toluene-sulfonic acid monohydrate in 200 ml glacial acetic acid were charged into a 1-L reaction vessel equipped with a paddle stirrer, reflux condenser and a nitrogen inlet tube. The mixture was heated to reflux and maintained at reflux to allow formation of the alternating copolymer. After 8 hours, 146.5 g salicylaldehyde were added over time to the reaction mixture to form substantially m-cresol-salicylaldehyde block segments. Reflux was continued for 8 hours. The reaction mixture was slowly poured into 7 L deionized water to precipitate the resin. Once the solvent had exchanged with water, the product was collected on a filter, slurried once in warm deionized water for about 30 minutes, again collected, rinsed with water and dried in a vacuum oven under about 125 mm Hg and at about 100 to 105° C. About 281 g of a block copolymer resin having a number average molecular weight, Mn, of 1472 Daltons and a Tg of 233° C. were obtained.

Quelle