Реакция #66751

ord-de58866a73cb48c7a016ae38f2f5ffeb

Уравнение реакции

CC(=O)c1cc(Br)ccc1O
5-bromo-2-hydroxyacetophenone
CC(C)(C)OC(=O)N1CCC(=O)CC1
N-Boc-piperidin-4-one
C1CCNC1
pyrrolidine
CO
MeOH
CC(C)(C)OC(=O)N1CCC2(CC1)CC(=O)c1cc(Br)ccc1O2
tert-Butyl 6-bromo-4-oxospiro[chroman-2,4′-piperidine]-1′-carboxylate

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураwas heated
  2. 2
    Температураunder reflux until the reaction
  3. 3
    ТемператураThe mixture was cooled
  4. 4
    Фильтрацияthe mixture was filtered
  5. 5
    Другоеdried
  6. 6
    Другоеto give

Методика

A mixture of 5-bromo-2-hydroxyacetophenone (104 g, 485 mmol), N-Boc-piperidin-4-one (98.6 g, 494 mmol), 20 mL of pyrrolidine (17.3 g, 243 mmol) and 261 mL of MeOH was heated under reflux until the reaction was complete. The mixture was cooled, then 87 mL of H2O were added, and the mixture was filtered and dried to give intended compound as a colorless solid.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08524730B2uspto-grants-2013_09