Hydrogen Bromide → HCID 5323829、化合物

HRID 1732857ノート

反応式

HRID 1732857 の反応式
[CH3:1][C:2]1[CH2:9][CH2:8][CH:7]=[C:6]([CH3:10])[CH2:5][CH2:4][CH:3]=1.CC1CCC(C)=CCCC=1.[BrH:21]>>[CH3:10][C:6]12[CH:3]([Br:21])[C:2]([CH3:1])([CH2:4][CH2:5]1)[CH2:9][CH2:8][CH2:7]2

参加物

4

反応物 3

HCID 260Hydrogen BromideHCID 773701,6-Dimethyl-1,5-cyclooctadieneHCID 773711,5-Dimethylcycloocta-1,5-diene

生成物 1

HCID 5323829HCID 5323829、化合物収率 93.3%

実験手順

A mixture of 68 g (0.5 mol) 1,5-dimethyl-1,5-cyclooctadiene and 1,6-dimethyl-1,5-cyclooctadiene (ratio 80/20) was boiled under stirring for 1 hour with 500 ml 48% hydrogen bromide and 10 g of AMBERLYST A15 ion-exchange resin. Thereafter, the reaction product was subjected to azeotrope distillation with the aqueous hydrogen bromide solution. The distillate was then extracted with pentane. The pentane layer was treated as described in Example 1a. By fractional distillation under reduced pressure 81 g 1,5-dimethyl-8-bromobicyclo[3,2,1]octane (b.p. 93° C./10 mm Hg) was obtained in 93.3% yield. The purity of the product according to gas-liquid chromatography was more than 98%.

後処理

  1. distillationdistillation with the aqueous hydrogen bromide solution
  2. extractionThe distillate was then extracted with pentane
  3. additionThe pentane layer was treated
  4. distillationBy fractional distillation under reduced pressure 81 g 1,5-dimethyl-8-bromobicyclo[3,2,1]octane (b.p. 93° C./10 mm Hg)
  5. customwas obtained in 93.3% yield

出典と根拠

ORDレコード
ord-b8268b6022a4445b8676f5c63c05a9d1
出典データセット
uspto-grants-1980_12
特許番号
US04239707

反応ノート

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