Phosphorus oxychloride → Pyridine-3-sulfonyl chloride

HRID 513366

반응식

HRID 513366 반응식
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

참가 물질

4

반응물 3

HCID 24813Phosphorus oxychlorideHCID 24819Phosphorus pentachlorideHCID 694683-Pyridinesulfonic acid

생성물 1

HCID 3164136Pyridine-3-sulfonyl chloride수율 36%

반응 조건

온도
130 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-750efa81a63c45cd9af11ee4b49a53ee
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09102688B2

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