반응 #335748

ord-75b02f6cafc54cccbd88e06e9e5b704c

반응 방정식

Brc1ccccc1Br
1,6-dibromobenzene
Clc1ccc(Cl)cc1
1,4-dichlorobenzene
C1CCOC1
tetrahydrofuran
Clc1ccc(CCCCCCBr)cc1
1-(6-bromohexyl)-4chlorobenzene
수율 45.0%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The full mixture was refluxed for 7 hours
  2. 2
    여과The precipitate was then filtered off
  3. 3
    기타the phases were separated
  4. 4
    세척The organic phase was washed
  5. 5
    기타dried
  6. 6
    기타evaporated

실험 절차

In the same manner as described in Example 1, a Grignard solution in a mixture containing 450 ml of toluene and 40 ml of tetrahydrofuran was prepared from 58.8 g (0.4 Mol) of 1,4-dichlorobenzene. A solution of 146.4 g (0.6 Mol) of commercially available 1,6-dibromobenzene in 100 ml of toluene and a catalytic amount of dilithium tetrachlorocuprate were added to this solution. The full mixture was refluxed for 7 hours. The precipitate was then filtered off, the filtrate was acidified, and the phases were separated. The organic phase was washed, dried and evaporated, and the residue was fractionated. About 50 g of 1-(6-bromohexyl)-4chlorobenzene (45 percent yield) were obtained at a pressure of 0.2 hPa and at 106° to 109° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05210247uspto-grants-1993_05