Phosphorus pentachloride → Pyridine-3-sulfonyl chloride

HRID 263845

反応式

HRID 263845 の反応式
[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

参加物

5

反応物 2

HCID 24819Phosphorus pentachlorideHCID 694683-Pyridinesulfonic acid

生成物 1

HCID 3164136Pyridine-3-sulfonyl chloride

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 1140Toluene溶媒

実験手順

3-pyridylsulfonic acid 5-5 (30 g, 0.188 mole) was added to PCl5 (46.8 g, 0.225 mole) suspended in 150 mL toluene and heated to reflux ovemight. 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 5-6 as a yellow oil that was used in the next step without purification. 1H NMR (300 MHz, CDCl3) a 9.27 (1H, s), 8.98 (1H, d, 8.35 (1H, d), 7.62 (1H, dd).

後処理

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

出典と根拠

ORDレコード
ord-02b5186211584d53996df20fcf1dd224
出典データセット
uspto-grants-1997_07
特許番号
US05646000

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