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

HRID 1253130ノート

反応式

HRID 1253130 の反応式
[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]

参加物

5

反応物 3

HCID 6366Vinylidene chlorideHCID 1363832-Chloro-2,3-dimethylbutaneHCID 6451240Aluminum(III) Chloride2 回

生成物 1

HCID 132952241,1-Dichloro-3,3,4-trimethylpent-1-ene収率 65%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
20 °C

実験手順

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##

後処理

  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

出典と根拠

ORDレコード
ord-863c4439291d4ced802e61be3e1e32d8
出典データセット
uspto-grants-1988_05
特許番号
US04747869

反応ノート

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