Phosphorus oxychloride → Pyridine-3-sulfonyl chloride

HRID 513366

反応式

HRID 513366 の反応式
P(Cl)(Cl)(Cl)(Cl)Cl.[N:7]1[CH:12]=[CH:11][CH:10]=[C:9]([S:13]([OH:16])(=O)=[O:14])[CH:8]=1.P(Cl)(Cl)([Cl:19])=O>>[N:7]1[CH:12]=[CH:11][CH:10]=[C:9]([S:13]([Cl:19])(=[O:16])=[O:14])[CH:8]=1

参加物

4

反応物 3

HCID 24813Phosphorus oxychlorideHCID 24819Phosphorus pentachlorideHCID 694683-Pyridinesulfonic acid

生成物 1

HCID 3164136Pyridine-3-sulfonyl chloride収率 36%

反応条件

温度
130 °C

実験手順

Phosphorus pentachloride (3.0 g, 14.6 mmol) was added to a solution of 3-pyridinesulfonic acid (1.5 g, 9.42 mmol) dissolved in phosphoryl trichloride (2.45 g, 16.0 mmol) and the mixture heated to 130° C. for 3 h under argon. The mixture was concentrated in vacuo, the residue was quenched over ice and extracted with ether. The organic phase was washed with a saturated sodium bicarbonate solution and concentrated in vacuo to give the crude title compound (0.6 g, 36%) which was used immediately without purification.

後処理

  1. concentrationThe mixture was concentrated in vacuo
  2. customthe residue was quenched over ice
  3. extractionextracted with ether
  4. washThe organic phase was washed with a saturated sodium bicarbonate solution
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-750efa81a63c45cd9af11ee4b49a53ee
出典データセット
uspto-grants-2015_08
特許番号
US09102688B2

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