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

HRID 128368

반응식

HRID 128368 반응식
[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

참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 16584PentachloropyridineHCID 517111Ammonium Carbonate

생성물 1

HCID 169902,3,5,6-Tetrachloropyridine수율 93.4%

시약·촉매·용매 3

HCID 23994Zinc촉매HCID 962Water용매HCID 7020607Dimethylmethanephosphonate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0520aea80ea34e55a0d5c85f8a28155c
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04259495

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