Reaktion #1057445

Reaktionsgleichung

poly(p-hydroxystyrene)

di-tert-butyl dicarbonate

pyridine

→

p-hydroxystyrene p-tert-butoxycarbonyloxystyrene

Lösungsmittel

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.DISSOLUTIONabout 1.05) was dissolved
2. 2
   Sonstigereacted at room temperature for 4 hours
3. 3
   Sonstigereaction solution
4. 4
   Einengenwas then concentrated under reduced pressure
5. 5
   workup.DISSOLUTIONby dissolving in 250 mL of acetone
6. 6
   workup.ADDITIONpoured into 3 L of water for precipitation
7. 7
   FiltrationThe thus deposited crystal was filtered off
8. 8
   Sonstigedried under reduced pressure

Vorschrift

In 250 mL of ethyl acetate, 50.0 g of poly(p-hydroxystyrene) (from Nippon Soda Co., Ltd.; weight average molecular weight (Mw) is about 15,000 and distribution (Mw/Mn) thereof about 1.05) was dissolved, then14.8 g of di-tert-butyl dicarbonate and 11.0 g of pyridine were added and reacted at room temperature for 4 hours. Said reaction solution was then concentrated under reduced pressure, followed by dissolving in 250 mL of acetone, then poured into 3 L of water for precipitation. The thus deposited crystal was filtered off and dried under reduced pressure to obtain 50.8 g of poly(p-hydroxystyrene/p-tert-butoxycarbonyloxystyrene) as a white powder crystal. The thus obtained crystal was named polymer A2. A composition ratio of p-hydroxystyrene unit and p-tert-butoxycarbonyloxystyrene unit in polymer A2 was found to be about 85:15 from the measurement results by 13CNMR. Weight average molecular weight (Mw) of polymer A2 was about 16,500 and distribution (Mw/Mn) thereof was about 1.05 from the measurement results by gel permeation chromatography using polystyrene as a standard.

Quelle