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Potassium Chloride → Benzene, 1,4-bis(phenylthio)-

HRID 1078704
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HRID 1078704 반응식
[C:1]1([S:7]([C:9]2[CH:14]=[CH:13][C:12]([S:15][C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)=[CH:11][CH:10]=2)=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.BrBr.[Cl-].[K+]>ClCCl>[C:16]1([S:15][C:12]2[CH:13]=[CH:14][C:9]([S:7][C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)=[CH:10][CH:11]=2)[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 4873Potassium ChlorideHCID 24408BromineHCID 18791838HCID 18791838, 화합물

생성물 1

HCID 626321Benzene, 1,4-bis(phenylthio)-

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

A 500-mL, round-bottom flask with a Teflon-covered magnetic stirring bar is charged with dichloromethane (50 mL), 10% KHCO3 (43 mL), and phenyl[4-(thiophenoxy)phenyl] sulfoxide (5 g, 17.0 mmol). To the reaction mixture is added bromine (2.72 g, 17.0 mmol) in dichloromethane (50 mL) over a period of 5 min with vigorous stirring. The reaction is continued for 30 min. To the reaction mixture is added a KCl saturated solution and dichloromethane (100 mL). The aqueous layer is extracted with dichloromethane (2×50 mL). The organic layer is washed with water, dried over anhydrous sodium sulfate, and filtered. After recrystallization from ether, the solid is obtained. The solid is dried under vacuum at room temperature for 20 h and then is used without further purification for polymerization.

후처리

  1. extractionThe aqueous layer is extracted with dichloromethane (2×50 mL)
  2. washThe organic layer is washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. customAfter recrystallization from ether
  6. customthe solid is obtained
  7. customThe solid is dried under vacuum at room temperature for 20 h
  8. customis used without further purification for polymerization

출처 및 근거

ORD 기록
ord-e40e783d14074e25945d5efa86c78a76
출처 데이터셋
uspto-grants-1996_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05550171

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