Hydrogen Peroxide → HCID 54398044，化合物

HRID 1753672笔记

反应方程式

HRID 1753672 反应方程式
[C:1]1([S:7][C:8]2[CH:13]=[CH:12][C:11]([C:14]([CH3:17])([CH3:16])[CH3:15])=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[OH:18]O.C1(C)C=CC=CC=1>C(O)(=O)C.O.O.O.O.O.S([O-])([O-])(=O)=S.[Na+].[Na+].O.C(OCC)(=O)C>[C:1]1([S:7]([C:8]2[CH:9]=[CH:10][C:11]([C:14]([CH3:17])([CH3:16])[CH3:15])=[CH:12][CH:13]=2)=[O:18])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参与物

8

反应物 3

HCID 784Hydrogen PeroxideHCID 1140甲苯HCID 114138224-叔丁基二苯硫醚

产物 1

HCID 54398044HCID 54398044，化合物收率 98%

试剂、催化剂与溶剂 4

HCID 61475五水硫代硫酸钠催化剂HCID 176醋酸溶剂HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂2 次HCID 8857乙酸乙酯溶剂

实验过程

In 160 g of acetic acid was dissolved 27.4 g of 4-tert-butylphenyl phenyl sulfide which had been synthesized according to the well-known formulation. While the solution was maintained at an internal temperature of 30° C., 9 g of 35 wt % aqueous hydrogen peroxide was added dropwise. The reaction solution was aged at room temperature for 18 hours, after which under ice cooling, a mixture of 1 g sodium thiosulfate pentahydrate and 50 g water was added dropwise to quench the reaction. The solution was combined with 200 g of toluene, 100 g of ethyl acetate, and 100 g of water. The organic layer was separated, washed with water, and concentrated in vacuum. This was followed by crystallization from hexane, filtration, and drying. There was obtained 25.4 g of the target compound, 4-tert-butylphenyl phenyl sulfoxide as white crystals. Yield 98%.

后处理

  1. customhad been synthesized
  2. additionwas added dropwise
  3. additionwas added dropwise
  4. customto quench
  5. customthe reaction
  6. customThe organic layer was separated
  7. washwashed with water
  8. concentrationconcentrated in vacuum
  9. customThis was followed by crystallization from hexane, filtration
  10. customdrying

来源与证据

ORD记录
ord-9103958332594fb8a77b685d9f7d5b60
来源数据集
uspto-grants-2015_10
专利号
US09164384B2

反应笔记

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