Phosphorus pentachloride → Pyridine-3-sulfonyl chloride

HRID 36649

반응식

HRID 36649 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([S:7]([OH:10])(=O)=[O:8])[CH:2]=1.P(Cl)(Cl)(Cl)(Cl)[Cl:12]>C1(C)C=CC=CC=1.C1C=CC=CC=1>[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([S:7]([Cl:12])(=[O:10])=[O:8])[CH:2]=1

참가 물질

5

반응물 2

HCID 24819Phosphorus pentachlorideHCID 694683-Pyridinesulfonic acid

생성물 1

HCID 3164136Pyridine-3-sulfonyl chloride수율 92%

시약·촉매·용매 2

HCID 241Benzene용매HCID 1140Toluene용매

실험 절차

3-Pyridylsulfonic acid (30 g, 0.188 mole) was added to PCl5 (46.8 g, 0.225 mole), suspended in 150 mL toluene and heated to reflux overnight. The suspension was cooled and concentrated to yield a yellow oil, which was diluted with benzene, filtered through a pad of celite and concentrated to give 30.7 g (92%) of 23-10 as a yellow oil, which was used in the next step without purification.

후처리

  1. temperatureheated
  2. temperatureto reflux overnight
  3. temperatureThe suspension was cooled
  4. concentrationconcentrated
  5. customto yield a yellow oil, which
  6. filtrationfiltered through a pad of celite
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-bf556213779245328caa8e5257c096ab
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05416099

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