Hydrochloric Acid → 5-Bromopyridine-3-sulphonic acid

HRID 839386ノート

反応式

HRID 839386 の反応式
[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

参加物

7

反応物 4

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

生成物 1

HCID 126842615-Bromopyridine-3-sulphonic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-fe469ed7e841436a912cd1202abd0cfd
出典データセット
uspto-grants-1978_06
特許番号
US04094982

反応ノート

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