반응 #414134

ord-3be182ec831b43929961dfec09d371a5

반응 방정식

C=CCCCCCCCCO
9-decene-1-ol
O=S(Cl)Cl
thionyl chloride
O=S(Cl)Cl
thionyl chloride
CCCCCCCCC=CCl
1-chloro-1-decene
수율 95.3%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the mixture was placed into an eggplant flask
  2. 2
    온도during cooling with ice
  3. 3
    기타After conclusion of the reaction
  4. 4
    세척washed with an aqueous potassium carbonate
  5. 5
    기타The washed solution was dried on magnesium sulfate
  6. 6
    농축concentrated under reduced pressure
  7. 7
    기타The resulting residue was purified by column chromatography

실험 절차

To 26.0 g of 9-decene-1-ol was added 10 drops of pyridine, and the mixture was placed into an eggplant flask. To the mixture was added dropwise 24.0 g of thionyl chloride, during cooling with ice. After dropping thionyl chloride, reaction was carried out for 8.5 hours at 70° C. After conclusion of the reaction, the reaction solution was diluted with dichloromethane, and then washed with an aqueous potassium carbonate. The washed solution was dried on magnesium sulfate, and then concentrated under reduced pressure. The resulting residue was purified by column chromatography to obtain 27.7 g of 1-chloro-1-decene. (Yield: 95%)

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05271866uspto-grants-1993_12