Phosphorus oxychloride → 93297-77-9

HRID 465125ノート

反応式

HRID 465125 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7]1[C:8](=O)[NH:9][CH:10]=[CH:11][CH:12]=1.P(Cl)(Cl)([Cl:16])=O>>[Cl:16][C:8]1[C:7]([C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][N:1]=2)=[CH:12][CH:11]=[CH:10][N:9]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 10419623HCID 10419623、化合物

生成物 1

HCID 1329872693297-77-9

実験手順

A 5.9 g portion of 3-(2-pyridinyl)-2(1H)-pyridinone in 100 ml of phosphorus oxychloride was heated on a steam bath for 18 hours, then concentrated under vacuum. The residue was stirred with crushed ice and chloroform and adjusted to pH 7 with 10N sodium hydroxide. The organic layer was separated, dried, filtered through a short pad of hydrous magnesium silicate and the filtrate concentrated under vacuum to an oil. This oil was heated with hexane, filtered while hot and the filtrate cooled to room temperature, giving 3.5 g of 2'-chloro-2,3'-bipyridine as white needles, mp 50° C.

後処理

  1. concentrationconcentrated under vacuum
  2. customThe organic layer was separated
  3. customdried
  4. filtrationfiltered through a short pad of hydrous magnesium silicate
  5. concentrationthe filtrate concentrated under vacuum to an oil
  6. temperatureThis oil was heated with hexane
  7. filtrationfiltered while hot and the filtrate

出典と根拠

ORDレコード
ord-2f1fb8ecee3f4c199c2ad8dc6fd94808
出典データセット
uspto-grants-1985_10
特許番号
US04550166

反応ノート

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