Vinylidene chloride → 1,1-Dichloro-3,3,4-trimethylpent-1-ene

HRID 1253130노트

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HRID 1253130 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[C:5]([Cl:8])([Cl:7])=[CH2:6].Cl[C:10]([CH3:15])([CH:12]([CH3:14])[CH3:13])[CH3:11]>C(O)(=O)C>[Cl:7][C:5]([Cl:8])=[CH:6][C:10]([CH3:15])([CH3:11])[CH:12]([CH3:14])[CH3:13]

참가 물질

5

반응물 3

HCID 6366Vinylidene chlorideHCID 1363832-Chloro-2,3-dimethylbutaneHCID 6451240Aluminum(III) Chloride2회

생성물 1

HCID 132952241,1-Dichloro-3,3,4-trimethylpent-1-ene수율 65%

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
20 °C

실험 절차

20 g of anhydrous, powdered aluminum chloride are added in portions to 2,040 g (21 mols) of vinylidene chloride at -10° C., in a dry apparatus equipped with a drying tube. 837 g (7 mols) of 2-chloro-2,3-dimethylbutane are then added dropwise in the temperature range from 0° to 10° C. The mixture is allowed to warm up to 20° C., and further aluminum chloride portions (a maximum of 20 g) are added, while cooling, until the reaction is no longer exothermic. The mixture is stirred for a further 4 hours at room temperature, the catalyst is deactivated by dropwise addition of 70 ml of acetic acid, and the mixture is filtered over sodium sulphate. The volatile constituents are separated from the sparingly volatile constituents by continuous-feed distillation under 1 mbar. The distillate is fractionated in a column. 824 g (65% of theory) of 1,1-dichloro-3,3,4-trimethyl-pent-1-ene of boiling point 60°-75° C./20 mbar are obtained. ##STR19##

후처리

  1. customequipped with a drying tube
  2. temperaturewhile cooling, until the reaction
  3. filtrationthe mixture is filtered over sodium sulphate
  4. customThe volatile constituents are separated from the sparingly volatile constituents by continuous-feed distillation under 1 mbar

출처 및 근거

ORD 기록
ord-863c4439291d4ced802e61be3e1e32d8
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04747869

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