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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Pentachloropyridine → 2,3,5,6-Tetrachloropyridine

HRID 128367
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HRID 128367 반응식
[Cl:1][C:2]1[N:7]=[C:6]([Cl:8])[C:5]([Cl:9])=[C:4](Cl)[C:3]=1[Cl:11].[Cl-].[NH4+]>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
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참가 물질

6

반응물 2

HCID 16584PentachloropyridineHCID 25517Ammonium Chloride2회

생성물 1

HCID 169902,3,5,6-Tetrachloropyridine수율 92.2%

시약·촉매·용매 3

HCID 23994Zinc촉매HCID 962Water용매HCID 7020607Dimethylmethanephosphonate용매

실험 절차

12.76 g (0.05 mol) of pentachloropyridine is dissolved, by heating at 90° C., in 80 ml of dimethylmethanephosphonate. After the addition of 4.1 g (0.063 gram atom) of zinc dust, there is added dropwise to the clear solution in the course of 20 minutes, with vigorous stirring, a solution of 4.26 g (0.08 mol) of ammonium chloride in 15 ml of water. After the addition of the ammonium chloride solution has been completed, stirring is continued for 40 minutes. The reaction mixture obtained is then filtered hot, and the filter residue is washed with 10 ml of dimethylmethanephosphonate. The filtrate is poured into 500 ml of ice water; there is then added 12.5 ml of concentrated hydrochloric acid and the mixture is stirred for 2 hours. The 2,3,5,6-tetrachloropyridine, which has precipitated in the form of white crystals, is subsequently washed with 150 ml of water and dried. In this manner is obtained 10.0 g (90.8% of theory) of 2,3,5,6 -tetrachloropyridine having a melting point of 89° to 90° C. According to gas-chromatographical analysis, the product contains 97.0% of 2,3,5,6-tetrachloropyridine, 0.5% of 2,3,5-trichloropyridine, 0.6% of 2,3,6-trichloropyridine and 1.6% of pentachloropyridine.

후처리

  1. additionis added dropwise to the clear solution in the course of 20 minutes, with vigorous stirring
  2. customThe reaction mixture obtained
  3. filtrationis then filtered hot
  4. washthe filter residue is washed with 10 ml of dimethylmethanephosphonate
  5. additionThe filtrate is poured into 500 ml of ice water
  6. additionthere is then added 12.5 ml of concentrated hydrochloric acid
  7. stirringthe mixture is stirred for 2 hours
  8. customThe 2,3,5,6-tetrachloropyridine, which has precipitated in the form of white crystals
  9. washis subsequently washed with 150 ml of water
  10. customdried

출처 및 근거

ORD 기록
ord-c9814b95be1b4f6e90daaf0dbd769fc7
출처 데이터셋
uspto-grants-1981_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04259495

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