Реакция #1563952

ord-315092a422724901a4e3efcc2ae85620

Растворители

Условия реакции

Температура
25°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеReaction mixture
  2. 2
    Другоеwas quenched with 1N aqueous HCl solution (50 mL)
  3. 3
    Экстракцияextracted with DCM (3×20 mL)
  4. 4
    СушкаThe organic layer was dried over anhydrous sodium sulphate
  5. 5
    Концентрированиеconcentrated under reduced pressure

Методика

NaBH4 (0.25 g, 6.69 mmol) was added to a solution of 5-(7-fluoro-2,3-dihydrobenzo[b][1,4]dioxin-5-yl)-3,4-dihydro-2H-pyrrole (Int-55) (0.8 g, 3.34 mmol) in a mixture of MeOH and H2O (3:1, 20 mL) and was stirred at 25° C. for 2 h. Reaction mixture was quenched with 1N aqueous HCl solution (50 mL) and basified with 2N aqueous NaOH solution to pH 8 and extracted with DCM (3×20 mL). The organic layer was dried over anhydrous sodium sulphate and concentrated under reduced pressure to afford 2-(7-fluoro-2,3-dihydrobenzo[b][1,4]dioxin-5-yl)pyrrolidine (Int-56). MS (ESI) m/z 224.5 (M+H).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09402833B2uspto-grants-2016_08