Hydrochloric Acid → 2,3,5,6-Tetrachloropyridine

HRID 128368

反応式

HRID 128368 の反応式
[Cl:1][C:2]1[N:7]=[C:6]([Cl:8])[C:5]([Cl:9])=[C:4](Cl)[C:3]=1[Cl:11].C(=O)([O-])[O-].[NH4+].[NH4+].Cl>CC(C)P([O-])(=O)[O-].O.[Zn]>[Cl:8][C:6]1[C:5]([Cl:9])=[CH:4][C:3]([Cl:11])=[C:2]([Cl:1])[N:7]=1

参加物

7

反応物 3

HCID 313Hydrochloric AcidHCID 16584PentachloropyridineHCID 517111Ammonium Carbonate

生成物 1

HCID 169902,3,5,6-Tetrachloropyridine収率 93.4%

試薬・触媒・溶媒 3

HCID 23994Zinc触媒HCID 962Water溶媒HCID 7020607Dimethylmethanephosphonate溶媒

実験手順

1.84 g (0.0281 gram atom) of zinc dust is introduced into a solution, heated to 80° C., of 5.1 g (0.02 mol) of pentachloropyridine in 35 ml of dimethylmethanephosphonate. A solution of 2.44 g (0.0254 mol) of ammonium carbonate in 10 ml of water is subsequently added dropwise at a temperature of 90° to 95° C. in the course of 70 minutes with vigorous stirring. The reaction mixture is then stirred into 250 ml of ice water; there is added 5 ml of concentrated hydrochloric acid and the mixture is stirred for a further 10 minutes, and is subsequently extracted twice with 100 ml of ether each time. The combined extracts are washed with 70 ml of water, dried over sodium sulfate, filtered, and evaporated to dryness to yield as residue 4.05 g (92% of theory) of 2,3,5,6-tetrachloropyridine having a melting point of 86° to 88° C. According to gas-chromatographical analysis, the product contains 93.4% of 2,3,5,6-tetrachloropyridine, 2.1% of 2,3,5-trichloropyridine, 2.2% of 2,3,6-trichloropyridine and 0.8% of pentachloropyridine.

後処理

  1. extractionis subsequently extracted twice with 100 ml of ether each time
  2. washThe combined extracts are washed with 70 ml of water
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. customevaporated to dryness

出典と根拠

ORDレコード
ord-0520aea80ea34e55a0d5c85f8a28155c
出典データセット
uspto-grants-1981_03
特許番号
US04259495

関連ノート

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