Hydrogen Peroxide → HCID 54398044, 화합물

HRID 1753672노트

반응식

HRID 1753672 반응식
[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

참가 물질

8

반응물 3

HCID 784Hydrogen PeroxideHCID 1140TolueneHCID 114138224-tert-Butyldiphenyl sulfide

생성물 1

HCID 54398044HCID 54398044, 화합물수율 98%

시약·촉매·용매 4

HCID 61475Sodium Thiosulfate Pentahydrate촉매HCID 176Acetic Acid용매HCID 962Water용매2회HCID 8857Ethyl Acetate용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-9103958332594fb8a77b685d9f7d5b60
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09164384B2

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