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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Diethyl Ether → HCID 46183783, 화합물

HRID 2369442
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HRID 2369442 반응식
[CH:1]1([C:4]#[C:5][C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=2[S:12][C:13]([F:16])([F:15])[F:14])[CH2:3][CH2:2]1.C(Cl)Cl.[F:20][C:21]([F:27])([F:26])[S:22]([OH:25])(=[O:24])=[O:23].CCOCC>C(#N)C>[O-:25][S:22]([C:21]([F:27])([F:26])[F:20])(=[O:24])=[O:23].[CH:1]1([C:4]2[S+:12]([C:13]([F:16])([F:14])[F:15])[C:7]3[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=3[CH:5]=2)[CH2:3][CH2:2]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 3283Diethyl EtherHCID 6344DichloromethaneHCID 62406Trifluoromethanesulfonic acidHCID 69670549HCID 69670549, 화합물

생성물 1

HCID 46183783HCID 46183783, 화합물수율 80.1%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
-50 °C

실험 절차

1-cyclopropylethynyl-2-trifluoromethylsulfanylbenzene (0.67 g, 2.77 mmol) prepared in Example 1 and anhydrous methylene chloride (5 ml) were charged into a 25-ml round-bottomed flask equipped with a stirrer, and cooled to −50° C. with stirring. To this mixture, trifluoromethanesulfonic acid (0.5 ml, 5.54 mmol) was added dropwise, and the solution was heated, and stirred at room temperature overnight. After completion of the reaction, a solvent was removed, ether (10 ml) was added to form a deposit, and the deposit was collected by filtration. The obtained crude product was dissolved in acetonitrile. After then, ether was added to form a precipitation, which was collected by filtration. This operation was repeated three times to purify the product. After the purification, target 2-cyclopropyl-1-trifluoromethylbenzo[b]thiophenyl triflate was obtained as a white solid (0.87 g, yield: 80%).

후처리

  1. customequipped with a stirrer
  2. temperaturethe solution was heated
  3. stirringstirred at room temperature overnight
  4. customAfter completion of the reaction
  5. customa solvent was removed
  6. additionether (10 ml) was added
  7. customto form a deposit
  8. filtrationthe deposit was collected by filtration
  9. customThe obtained crude product
  10. customto form
  11. customa precipitation, which
  12. filtrationwas collected by filtration
  13. customto purify the product
  14. customAfter the purification

출처 및 근거

ORD 기록
ord-710358278c9542189755cf16997cab32
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08703969B2

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