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Chloride → HCID 20505900, 화합물

HRID 1730603
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HRID 1730603 반응식
[Cl:1][C:2]1[CH:10]=[CH:9][C:8]([S:11](Cl)(=[O:13])=[O:12])=[C:7]([Cl:15])[C:3]=1[C:4]([OH:6])=[O:5].[NH:16]1[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1.[Cl-]>>[Cl:1][C:2]1[CH:10]=[CH:9][C:8]([S:11]([N:16]2[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]2)(=[O:13])=[O:12])=[C:7]([Cl:15])[C:3]=1[C:4]([OH:6])=[O:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 312ChlorideHCID 8082PiperidineHCID 35382162,6-Dichloro-3-(chlorosulfonyl)benzoic acid

생성물 1

HCID 20505900HCID 20505900, 화합물

실험 절차

2,6-Dichloro-5-chlorosulfonylbenzoic acid (960 mg.; 3.3 m moles) is added portion-wise to 1.95 g. (0.0165 mole) of piperidine in 15 ml. of drymethylene chloride, and the mixture heated to reflux for 1.5 hrs. The solvent and excess amine are removed under reduced pressure and the residue dissolved in 15 ml. of 2N sodium hydroxide. The aqueous base solution is extracted (2 x 50 ml.) with ether and acidified with 6N hydrochloric acid. The precipitated gum is filtered, dried and allowed to crystallize in hexane, 1.1 g., m.p. 145°-150° C. A small sample is recrystallized from acetonitrile, m.p. 142°-145° C.

후처리

temperature
to reflux for 1.5 hrs
  • customThe solvent and excess amine are removed under reduced pressure
  • dissolutionthe residue dissolved in 15 ml
  • extractionThe aqueous base solution is extracted (2 x 50 ml.) with ether
  • filtrationThe precipitated gum is filtered
  • customdried
  • customto crystallize in hexane
  • customA small sample is recrystallized from acetonitrile, m.p. 142°-145° C.
  • 출처 및 근거

    ORD 기록
    ord-aaab80451448491684ac4331af6d0602
    출처 데이터셋
    uspto-grants-1976_11
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US03992441

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