碘化钾 → Bis[4-(2-methoxyethoxy)phenyl]sulfide

HRID 1753683

反应方程式

HRID 1753683 反应方程式
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][C:9]2[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=2)=[CH:4][CH:3]=1.[CH3:16][O:17][CH2:18][CH2:19]Cl.[C:21](=[O:24])([O-])[O-].[K+].[K+].[I-].[K+].[CH3:29][CH2:30]CCCC>C1(C)C=CC=CC=1.O.CN(C=O)C>[CH3:16][O:17][CH2:18][CH2:19][O:15][C:12]1[CH:13]=[CH:14][C:9]([S:8][C:5]2[CH:6]=[CH:7][C:2]([O:1][CH2:29][CH2:30][O:24][CH3:21])=[CH:3][CH:4]=2)=[CH:10][CH:11]=1

参与物

9

反应物 5

HCID 4875碘化钾HCID 8058正己烷HCID 11430碳酸钾HCID 123162-氯乙基甲基醚HCID 175704,4'-二羟基二苯硫醚

产物 1

HCID 117666858Bis[4-(2-methoxyethoxy)phenyl]sulfide收率 74%

试剂、催化剂与溶剂 3

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂HCID 1140甲苯溶剂HCID 6228N,N-二甲基甲酰胺溶剂

实验过程

A solution was prepared by combining 25.0 g of bis(4-hydroxyphenyl) sulfide, 20.7 g of 2-chloroethyl methyl ether, 31.7 g of potassium carbonate, 3.62 g of potassium iodide, and 50 g of DMF. The solution was aged at 80° C. for 1 week. Under ice cooling, 50 g of water was added to the solution to quench the reaction. To the solution, 50 g of toluene and 50 g of hexane were added. The organic layer was separated and washed with water. On subsequent concentration in vacuum, 28.5 g of the target compound, bis[4-(2-methoxy-ethoxy)phenyl]sulfide was obtained as oily matter. Yield 74%.

后处理

  1. customA solution was prepared
  2. waitThe solution was aged at 80° C. for 1 week
  3. customto quench
  4. customthe reaction
  5. customThe organic layer was separated
  6. washwashed with water
  7. concentrationOn subsequent concentration in vacuum, 28.5 g of the target compound

来源与证据

ORD记录
ord-674442f387cb4ff8923bc7221ba5fd59
来源数据集
uspto-grants-2015_10
专利号
US09164384B2

关联笔记

加载中…