HRID443020

反应详情

EQUATION

反应方程式

HRID 443020 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

375 g (1.65 mol) of 4-(2,3-epoxypropoxy)-1,2,2,6,6-pentamethylpiperidine (=A1a) in 1.51 of xylene are introduced under argon into a 2.5 l sulfonation flask fitted with magnetic stirrer, thermometer and condenser. 108 g (1.5 mol) of acrylic acid and 27.8 g (75 mmol) of ethyltriphenylphosphonium bromide are added. The reactants are allowed to react at 70° C. for 18 hours. The cooled product is poured into ice water, and the organic phase is separated off, washed twice with 1N sodium hydroxide solution, dried and evaporated. The residue is distilled over a short Vigreux column. 193 g (43%) of the title product are obtained as a clear liquid of boiling point 119-125° C. (0.06 mmHg).

WORKUP

后处理

  1. customfitted with magnetic stirrer
  2. customto react at 70° C. for 18 hours
  3. customthe organic phase is separated off
  4. washwashed twice with 1N sodium hydroxide solution
  5. customdried
  6. customevaporated
  7. distillationThe residue is distilled over a short Vigreux column