卡波姆树脂 → 1-Butanaminium, N,N,N-tributyl-, 2-propenoate (1:1)

HRID 22042

反应方程式

HRID 22042 反应方程式
[C:1]([OH:5])(=[O:4])[CH:2]=[CH2:3].[OH-].[CH2:7]([N+:11]([CH2:20][CH2:21][CH2:22][CH3:23])([CH2:16][CH2:17][CH2:18][CH3:19])[CH2:12][CH2:13][CH2:14][CH3:15])[CH2:8][CH2:9][CH3:10]>>[C:1]([O-:5])(=[O:4])[CH:2]=[CH2:3].[CH2:20]([N+:11]([CH2:7][CH2:8][CH2:9][CH3:10])([CH2:12][CH2:13][CH2:14][CH3:15])[CH2:16][CH2:17][CH2:18][CH3:19])[CH2:21][CH2:22][CH3:23]

参与物

3

反应物 2

HCID 6581卡波姆树脂HCID 2723671四丁基氢氧化铵

产物 1

HCID 30149221-Butanaminium, N,N,N-tributyl-, 2-propenoate (1:1)

反应条件

温度
65 °C

实验过程

A 5 liter glass reaction vessel, fitted with a magnetic stirrer, a hose connector, and a septum were purged with nitrogen. Operating in an atmosphere of nitrogen, 297 grams of poly(isobutylene-co-parabromomethylstyrene) (Mv=1.2M, 1.7% para-bromomethylstyrene) was placed into the vessel along with 3.5 liters of xylenes. The polymer was dissolved with stirring under a partial vacuum of 100 mm Hg with a nitrogen sparge attached at the bottom of the solution. A xylene solution of tetrabutylammonium acrylate was prepared in a second flask under nitrogen by placing 100 ml xylenes, 60 ml tetrabutylammonium hydroxide (1M in methanol) and 6.0 g acrylic acid together with stirring. The contents of the flask was concentrated to half its volume and then diluted to 0.5 liters with more xylenes. This solution was then added to the flask containing the poly(isobutylene-co-para-bromomethylstyrene) and the temperature of the solution was raised to 65° C. The reaction was complete in six hours and the polymer was isolated by precipitation in isopropanol. The polymer was dried in a vacuum oven at 1 mm Hg, 40° C. The analysis for the acrylate content (FTIR and NMR) indicate that the modified polymer has 0.24 meq/gram which is consistent with the complete conversion of acrylic acid to acrylic ester and total conversion of the benzylbromide.

后处理

  1. customfitted with a magnetic stirrer
  2. customa hose connector, and a septum were purged with nitrogen
  3. dissolutionThe polymer was dissolved
  4. customsparge
  5. stirringwith stirring
  6. concentrationThe contents of the flask was concentrated to half its volume
  7. additiondiluted to 0.5 liters with more xylenes
  8. additionThis solution was then added to the flask
  9. additioncontaining the poly(isobutylene-co-para-bromomethylstyrene)
  10. customthe polymer was isolated by precipitation in isopropanol
  11. customThe polymer was dried in a vacuum oven at 1 mm Hg, 40° C

来源与证据

ORD记录
ord-687d7e275b804438aca088ce635be0aa
来源数据集
uspto-grants-1995_06
专利号
US05426167

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