2,2’-[(1-甲基亚乙基)二(4,1-亚苯基氧亚甲基)]二环氧乙烷与α-氢-ω-羟基聚(氧-1,2-亚乙基)的聚合物 → 2-(3-溴-4-氟苯基)-1,3-二氧戊环

HRID 34603

反应方程式

HRID 34603 反应方程式
[Br:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[F:10])[CH:5]=[O:6].[CH2:11](O)[CH2:12][OH:13]>C1(C)C=CC(S(O)(=O)=O)=CC=1.C1(C)C=CC=CC=1>[Br:1][C:2]1[CH:3]=[C:4]([CH:5]2[O:13][CH2:12][CH2:11][O:6]2)[CH:7]=[CH:8][C:9]=1[F:10]

参与物

5

反应物 2

HCID 1742,2’-[(1-甲基亚乙基)二(4,1-亚苯基氧亚甲基)]二环氧乙烷与α-氢-ω-羟基聚(氧-1,2-亚乙基)的聚合物HCID 1736043-溴-4-氟苯甲醛

产物 1

HCID 109777652-(3-溴-4-氟苯基)-1,3-二氧戊环收率 78.3%

试剂、催化剂与溶剂 2

HCID 6101对甲苯磺酸催化剂HCID 1140甲苯溶剂

实验过程

A mixture of 3-bromo-4-fluorobenzaldehyde (45.7 g), ethylene glycol (27.39 g), p-toluenesulphonic acid (0.225 g) and dry toluene (110 cm3) was heated at the reflux temperature under a Dean and Stark trap. After 4.5 hours, approximately 12 cm3 of water had collected in the trap, and analysis of the reaction mixture by gas liquid chromatography indicated that no starting aldehyde was present. The mixture was washed with sodium bicarbonate solution and brine, and dried over anhydrous magnesium sulphate. Evaporation of the solvent under reduced pressure gave a yellow oil, which was purified by distillation under reduced pressure to give 2-(3-bromo-4-fluorophenyl)-1,3-dioxolane (43.56 g), boiling point 68°-106° C. at 0.04 mmHg.

后处理

  1. temperaturewas heated at the reflux temperature under a Dean and Stark trap
  2. customapproximately 12 cm3 of water had collected in the trap, and analysis of the reaction mixture by gas liquid chromatography
  3. washThe mixture was washed with sodium bicarbonate solution and brine
  4. dry with materialdried over anhydrous magnesium sulphate
  5. customEvaporation of the solvent under reduced pressure
  6. customgave a yellow oil, which
  7. distillationwas purified by distillation under reduced pressure

来源与证据

ORD记录
ord-c060ac6cc12e4d48b786ab94b72b761c
来源数据集
uspto-grants-1988_08
专利号
US04762835

关联笔记

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