Reaktion #465381

ord-b097b090a3c541ebbc2a013b8f37936f

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas added to the solution
  2. 2
    Waschenwas washed in 3% solution of Na2CO3, saturated water of salt and water in this order
  3. 3
    Trocknenthe organic layer was dried with MgSO4
  4. 4
    SonstigeWhen ether and residual 3,4-dihydro-2H-pyran were removed in vacuum
  5. 5
    Sonstigean evaporator, we

Vorschrift

Subsequently, carboxyhexacyclo[6.6.1.13,6.110,13.02,7.09,14 ]heptadecen of 2.1 grams and 3,4-dihydro-2H-pyran of 1.71 grams were dissolved in tetrahydrofuran of 50 milli-litter, and p-toluen sulfonic acid of 0.03 gram was added to the solution. The reaction was continued at room temperature for 2 hours. The resultant material was diluted in ether of 100 milli-litter, and was washed in 3% solution of Na2CO3, saturated water of salt and water in this order, and the organic layer was dried with MgSO4. When ether and residual 3,4-dihydro-2H-pyran were removed in vacuum by using an evaporator, we obtained viscous-liquid of 12-tetrahydropyranyloxycarbonilhexacyclo[6.6.1.13,6.110,13.02,7.09,14 ]heptadecen of 2 grams.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06030747uspto-grants-2000_02