Hydrochloric Acid → 4-Methyl-2,2-dichloro-1,3-benzodioxole

HRID 476975

反応式

HRID 476975 の反応式
[CH3:1][C:2]1[C:10]2[O:9][CH2:8][O:7][C:6]=2[CH:5]=[CH:4][CH:3]=1.P(Cl)(Cl)(Cl)(Cl)Cl.[ClH:17].[Cl:18]Cl>C(Cl)(Cl)(Cl)Cl>[CH3:1][C:2]1[C:10]2[O:9][C:8]([Cl:18])([Cl:17])[O:7][C:6]=2[CH:5]=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 24526ChlorineHCID 24819Phosphorus pentachlorideHCID 885604-Methyl-1,3-benzodioxole

生成物 1

HCID 144051544-Methyl-2,2-dichloro-1,3-benzodioxole

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

160 g of 4-methyl-1,3-benzodioxole are added dropwise to 276 g of phosphorus pentachloride in 840 ml of carbon tetrachloride (prepared from phosphorus trichloride and chlorine), with stirring. Vigorous evolution of hydrogen chloride starts immediately. Towards the end of the reaction, 85 g of chlorine are passed in at about 20° C. and when the evolution of gas has ended, the mixture is then heated under reflux. By distillation, the phosphorus trichloride and carbon tetrachloride are recovered and the 4-methyl-2,2-dichloro-1,3-benzodioxole is then obtained at boiling point: 98-99° C. (22 mbar).

後処理

  1. customare passed in at about 20° C. and when
  2. temperaturethe mixture is then heated
  3. temperatureunder reflux
  4. distillationBy distillation
  5. customthe phosphorus trichloride and carbon tetrachloride are recovered

出典と根拠

ORDレコード
ord-0ce8641352074532a813a695ba1e500a
出典データセット
uspto-grants-1989_12
特許番号
US04886816

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