海萝胶 → m-Bromophenyl 3-methyl-2-butenyl sulfide

HRID 37404

反应方程式

HRID 37404 反应方程式
[Br:1][C:2]1[CH:3]=[C:4]([SH:8])[CH:5]=[CH:6][CH:7]=1.C(=O)([O-])[O-].[K+].[K+].[CH3:15][C:16]([CH3:20])=[CH:17][CH2:18]Br.Cl>CN(C)C=O.O>[CH3:15][C:16]([CH3:20])=[CH:17][CH2:18][S:8][C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([Br:1])[CH:3]=1

参与物

7

反应物 4

HCID 313海萝胶HCID 11430碳酸钾HCID 700921-溴-3-甲基-2-丁烯HCID 805973-溴苯硫酚

产物 1

HCID 22640690m-Bromophenyl 3-methyl-2-butenyl sulfide收率 98%

试剂、催化剂与溶剂 2

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂HCID 6228N,N-二甲基甲酰胺溶剂

实验过程

36 g of 3-bromothiophenol were dissolved in 400 ml of dimethylformamide. After the addition of 27 g of finely powdered potassium carbonate and 29 g of 3,3-dimethylallyl bromide, the mixture was stirred at room temperature for 1 hour, diluted with 500 ml of water, acidified with 3N hydrochloric acid while cooling and extracted with ether. The yellow-brown oil obtained after evaporation was distilled in a high vacuum. There were obtained 48 g of m-bromophenyl 3-methyl-2-butenyl sulfide as a colorless liquid, boiling point 85° C./13.3 Pa.

后处理

  1. temperaturewhile cooling
  2. extractionextracted with ether
  3. customThe yellow-brown oil obtained
  4. customafter evaporation
  5. distillationwas distilled in a high vacuum

来源与证据

ORD记录
ord-6a109ae7194e4a79adaf25d9e834a073
来源数据集
uspto-grants-1995_05
专利号
US05420273

关联笔记

加载中…