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Cyclopropyldiphenylsulphonium tetrafluoroborate → Cyclopropyldiphenylsulfonium 2-naphthalene sulfonate

HRID 1413757
노트
인쇄 미리보기

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HRID 1413757 반응식
F[B-](F)(F)F.[CH:6]1([S+:9]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH2:8][CH2:7]1.[CH:22]1[C:31]2[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=2)[CH:25]=[CH:24][C:23]=1[S:32]([O-:35])(=[O:34])=[O:33].[K+]>O>[CH:6]1([S+:9]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH2:8][CH2:7]1.[CH:22]1[C:31]2[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=2)[CH:25]=[CH:24][C:23]=1[S:32]([O-:35])(=[O:34])=[O:33]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 2724210Cyclopropyldiphenylsulphonium tetrafluoroborateHCID 23670145Potassium naphthalene-2-sulfonate

생성물 1

HCID 20290499Cyclopropyldiphenylsulfonium 2-naphthalene sulfonate

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
90 °C

실험 절차

5.0 g. of cyclopropyl diphenyl sulfonium tetrafluoroborate is dissolved in 30 ml. water by heating the solution to 90°-95° C. To this is added 50 ml. of a hot solution of potassium naphthalene-2-sulfonate (obtained by heating 49.7 g. of naphthalene-2-sulfonic acid and 12 g. potassium hydroxide in 100 ml. water). The above reaction mixture is then mixed vigorously and maintained at 90° C. for a few minutes and then allowed to cool gradually to room temperature. The reaction mixture is then filtered free of any precipitate and the aqueous filtrate extracted several times with methylene chloride. The combined methylene chloride extracts, after drying over sodium sulphate, is filtered and evaporated i.v. to dryness. The residue is triturated with ether to obtain the title compound, m.p. 93°-95° C.

후처리

  1. additionTo this is added 50 ml
  2. customThe above reaction mixture
  3. additionis then mixed vigorously
  4. temperatureto cool gradually to room temperature
  5. filtrationThe reaction mixture is then filtered free of any precipitate
  6. extractionthe aqueous filtrate extracted several times with methylene chloride
  7. dry with materialafter drying over sodium sulphate
  8. filtrationis filtered
  9. customevaporated i.v
  10. customThe residue is triturated with ether

출처 및 근거

ORD 기록
ord-de25df93a37841cbbafcb5094a69a3a4
출처 데이터셋
uspto-grants-1981_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04251521

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