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Diethyl Ether → HCID 46224324、化合物

HRID 2369445
ノート
印刷プレビュー

反応式

HRID 2369445 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 3283Diethyl EtherHCID 62406Trifluoromethanesulfonic acidHCID 46224400HCID 46224400、化合物

生成物 1

HCID 46224324HCID 46224324、化合物収率 80%

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
-80 °C

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-7f539fca86644e94a37fbf7afdd281cd
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08703969B2

反応ノート

読み込み中…

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