HRID970263

反应详情

EQUATION

反应方程式

HRID 970263 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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.

WORKUP

后处理

  1. dissolutionabout 1.05) was dissolved
  2. customreacted at room temperature for 4 hours
  3. customreaction solution
  4. concentrationwas then concentrated under reduced pressure
  5. dissolutionby dissolving in 250 mL of acetone
  6. additionpoured into 3 L of water for precipitation
  7. filtrationThe thus deposited crystal was filtered off
  8. customdried under reduced pressure