Реакция #473780

ord-f661c0a74a9c41aea1d7d3d666c0fe8f

Растворители

Условия реакции

Температура
80°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONeach added three times
  2. 2
    workup.STIRRINGin each case the mixture is stirred for several hours at 80° C
  3. 3
    ТемператураThe reaction mixture is cooled
  4. 4
    Фильтрацияfiltered
  5. 5
    Промывкаwashed with water
  6. 6
    Другоеdried

Методика

16.0 g potassium carbonate and 20.0 g 8-methanesulphonyloxy-1,4-dioxa-spiro[4.5]decan are added at 50° C. to 20.0 g 3-benzyl-3,4-dihydro-4-oxo-6-hydroxy-7-methoxy-quinazoline in 150 ml N,N-dimethylformamide and the mixture is vigorously stirred for 18 hours at 80° C. To complete the reaction potassium carbonate and 8-methanesulphonyloxy-1,4-dioxa-spiro[4.5]decan are each added three times and in each case the mixture is stirred for several hours at 80° C. The reaction mixture is cooled and slowly combined with a total of 500 ml of water. The precipitate is suction filtered, washed with water and dried.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08372855B2uspto-grants-2013_02