Hydrochloric Acid → 5-Bromopyridine-3-sulphonic acid

HRID 839386노트

반응식

HRID 839386 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([S:7]([OH:10])(=[O:9])=[O:8])[CH:2]=1.P(Cl)(Cl)(Cl)(Cl)Cl.Cl.[Br:18]Br>O.C(Cl)(Cl)Cl>[Br:18][C:5]1[CH:4]=[C:3]([S:7]([OH:10])(=[O:9])=[O:8])[CH:2]=[N:1][CH:6]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 24408BromineHCID 24819Phosphorus pentachlorideHCID 694683-Pyridinesulfonic acid

생성물 1

HCID 126842615-Bromopyridine-3-sulphonic acid

시약·촉매·용매 2

HCID 962Water용매HCID 6212Chloroform용매

실험 절차

A mixture of 3g. of 3-pyridinesulfonic acid and 8.5g. of phosphorous pentachloride was heated at 120° C for 1.5 hours. Upon cooling to room temperature, the mixture solidified. Chloroform was added thereto and dry hydrogen chloride gas was introduced. The resulting precipitate was collected by filtration and dried. The crystalline substance obtained was heated with bromine (4g.) at 120° C. for 8 hours and water (60 ml.) was added to the mixture. After stirring at 80° C. for 2 hours, the solution was concentrated. On addition of acetone, 2g. of 5-bromo- 3-pyridinesulfonic acid was obtained.

후처리

  1. filtrationThe resulting precipitate was collected by filtration
  2. customdried
  3. customThe crystalline substance obtained
  4. concentrationthe solution was concentrated
  5. additionOn addition of acetone, 2g

출처 및 근거

ORD 기록
ord-fe469ed7e841436a912cd1202abd0cfd
출처 데이터셋
uspto-grants-1978_06
특허 번호
US04094982

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