Dibutylamine → N-(1,3-dithiol-2-ylidene)-N,N-di(n-butyl)ammonium perchlorate

HRID 648908ノート

反応式

HRID 648908 の反応式
[Cl:1]([O-:5])(=[O:4])(=[O:3])=[O:2].CS[C:8]1[S:12][CH:11]=[CH:10][S+:9]=1.[CH2:13]([NH:17][CH2:18][CH2:19][CH2:20][CH3:21])[CH2:14][CH2:15][CH3:16]>O1CCCC1>[Cl:1]([O-:5])(=[O:4])(=[O:3])=[O:2].[S:9]1[CH:10]=[CH:11][S:12][C:8]1=[N+:17]([CH2:18][CH2:19][CH2:20][CH3:21])[CH2:13][CH2:14][CH2:15][CH3:16]

参加物

4

反応物 2

HCID 8148DibutylamineHCID 230390092-Methylthio-1,3-dithiolium perchlorate

生成物 1

HCID 14127443N-(1,3-dithiol-2-ylidene)-N,N-di(n-butyl)ammonium perchlorate収率 75%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To 10 ml of tetrahydrofuran, 2.0 g of 2-methylthio-1,3-dithiolium perchlorate was suspended, and 0.75 ml of dibutylamine was dropwise added over a period of 5 minutes. The mixture was stirred at room temperature for 30 minutes, and the solvent was distilled off under reduced pressure. The residue was dissolved in a mixture of acetone-ethyl ether, and cooled to -70° C. in a cooling medium, whereupon crystals precipitated. The crystals were collected by decantation under cooled condition, and purified by liquid chromatography (column: Senshu pack, Senshu ODS-5301, mobile phase: methanol/water=50/50), whereby 0.20 g (yield: 75%) of N-(1,3-dithiol-2-ylidene)-N,N-di(n-butyl)ammonium perchlorate was obtained as oily substance. (Compound No. 23)

後処理

  1. distillationthe solvent was distilled off under reduced pressure
  2. dissolutionThe residue was dissolved in a mixture of acetone-ethyl ether
  3. temperaturecooled to -70° C. in a cooling medium, whereupon crystals
  4. customprecipitated
  5. customThe crystals were collected by decantation
  6. temperatureunder cooled condition
  7. custompurified by liquid chromatography (column: Senshu pack, Senshu ODS-5301, mobile phase: methanol/water=50/50)

出典と根拠

ORDレコード
ord-3b5ce801c6e0432da8cca301aba6091e
出典データセット
uspto-grants-1988_04
特許番号
US04737494

反応ノート

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