Hydrochloric Acid → 2,6-Dichloro-4-(dichloromethyl)pyridine

HRID 461441

반응식

HRID 461441 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([C:8](Cl)([Cl:10])[Cl:9])[CH:5]=[C:4]([Cl:12])[N:3]=1.Cl>CC(C)=O>[Cl:1][C:2]1[CH:7]=[C:6]([CH:8]([Cl:9])[Cl:10])[CH:5]=[C:4]([Cl:12])[N:3]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 897822,6-Dichloro-4-(trichloromethyl)pyridine

생성물 1

HCID 205177012,6-Dichloro-4-(dichloromethyl)pyridine

시약·촉매·용매 1

HCID 180Acetone용매2회

실험 절차

To a solution of 73 grams (0.275 mole) of 2,6-dichloro-4-(trichloromethyl)pyridine dissolved in 125 milliliters of acetone was added a solution of 108 grams (0.48 mole) of stannous chloride hydrate and 40 milliliters of concentrated hydrochloride acid in 500 milliliters of acetone. The mixture was refluxed for 2.0 hours. The solid which formed was separated by filtration and three fourths of the solvent was thereafter removed by evaporation. The remainder of the reaction mixture was diluted with water and the oil phase which formed, removed by extraction with hexane. The 2,6-dichloro-4-(dichloromethyl)pyridine product was dried and recovered from the solvent by evaporation of the solvent. The product had a boiling point of 123°- 126° C. at 1.6 millimeters of mercury.

후처리

  1. temperatureThe mixture was refluxed for 2.0 hours
  2. customThe solid which formed
  3. customwas separated by filtration and three fourths of the solvent
  4. customwas thereafter removed by evaporation
  5. additionThe remainder of the reaction mixture was diluted with water
  6. customthe oil phase which formed
  7. customremoved by extraction with hexane
  8. dry with materialThe 2,6-dichloro-4-(dichloromethyl)pyridine product was dried
  9. customrecovered from the solvent by evaporation of the solvent

출처 및 근거

ORD 기록
ord-553d0285329740668b77adfb8afd6475
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04062962

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