Reaktion #43971

ord-9de6be5db1d64bdda81b15f117fd822a

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAt 3.7 hours after the initiation of the reaction
  2. 2
    workup.ADDITIONThen the addition
  3. 3
    Sonstigeafter the initiation of the reaction
  4. 4
    Sonstigeis separated so that an oil layer
  5. 5
    workup.ADDITIONfor adding total amount of 459 g of allyl chloride
  6. 6
    workup.WAITwas 8 hours
  7. 7
    Sonstigeafter the initiation of the reaction
  8. 8
    workup.WAITwas 11 hours
  9. 9
    Sonstigeafter the initiation of the reaction
  10. 10
    Sonstigewas between 70° C. and 90° C
  11. 11
    workup.WAITAfter the mixture was digested for one hour
  12. 12
    Temperaturthe mixture was cooled

Vorschrift

At 3.7 hours after the initiation of the reaction, the addition of 200 g of allyl chloride was completed. Then the addition was continued. The time required for adding 300 g of allyl chloride was 5.5 hours after the initiation of the reaction. At this point of time (at the time at which allyl halide was added in the amount of 20% by mol, based on total molar number of hydroxyl group contained in D-sorbitol), the reflux liquid is separated so that an oil layer alone is returned to the reactor by attaching a water metering reservoir between the reflux condenser and the reactor. The time required for adding total amount of 459 g of allyl chloride was 8 hours after the initiation of the reaction. At this point of time, the dropwise addition of 333 g of 48% aqueous sodium hydroxide solution from the other dropping funnel was initiated. The time required for adding total amount of 842 g of allyl chloride was 11 hours after the initiation of the reaction. The temperature was between 70° C. and 90° C. After the mixture was digested for one hour, the mixture was cooled.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07732646B2uspto-grants-2010_06