Hydrogen Bromide → HCID 5323829, 화합물

HRID 1732857노트

반응식

HRID 1732857 반응식
[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

참가 물질

4

반응물 3

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

생성물 1

HCID 5323829HCID 5323829, 화합물수율 93.3%

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-b8268b6022a4445b8676f5c63c05a9d1
출처 데이터셋
uspto-grants-1980_12
특허 번호
US04239707

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