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Diethyl Ether → HCID 46224324, 화합물

HRID 2369445
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HRID 2369445 반응식
[F:1][C:2]([S:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[C:12]#[C:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)([F:4])[F:3].[F:20][C:21]([F:27])([F:26])[S:22]([OH:25])(=[O:24])=[O:23].CCOCC>C(Cl)Cl.C(#N)C>[F:20][C:21]([F:27])([F:26])[S:22]([O-:25])(=[O:24])=[O:23].[F:1][C:2]([F:4])([F:3])[S+:5]1[C:13]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[CH:12][C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]1=2
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참가 물질

6

반응물 3

HCID 3283Diethyl EtherHCID 62406Trifluoromethanesulfonic acidHCID 46224400HCID 46224400, 화합물

생성물 1

HCID 46224324HCID 46224324, 화합물수율 80%

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 6344Dichloromethane용매

반응 조건

온도
-80 °C

실험 절차

A solution of (trifluoromethyl)-(2-(2-phenylethynyl)phenyl)sulfide (1.5 g, 5.4 mmol) prepared in Example 2 in 10 ml of methylene chloride was charged into a 50-ml eggplant flask equipped with a stirrer, and cooled to −80° C. Then, trifluoromethanesulfonic acid (1.62 g, 10.8 mmol) was added dropwise to the solution, and the solution was gradually heated to room temperature, and stirred overnight. After completion of the reaction, a solvent was removed, ether was added to the obtained residue to cause solidification, and the solidified product was filtered and washed with ether. The obtained crude product was dissolved in acetonitrile, and ether was added to the solution to cause crystallization to obtain target S-(trifluoromethyl)-2-phenylbenzo[b]thiophenium trifluoromethanesulfonate (1.8 g, 80%).

후처리

  1. customequipped with a stirrer
  2. temperaturethe solution was gradually heated to room temperature
  3. customAfter completion of the reaction
  4. customa solvent was removed
  5. additionether was added to the obtained residue
  6. filtrationthe solidified product was filtered
  7. washwashed with ether
  8. customThe obtained crude product
  9. customcrystallization

출처 및 근거

ORD 기록
ord-7f539fca86644e94a37fbf7afdd281cd
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08703969B2

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