Reacción #166413

ord-ab295fc97e9f47a881009d73c7510aad

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    TemperaturaAfter 1.25 hours of reflux the reaction
  2. 2
    Otroquenched with water (2.22 mL)
  3. 3
    FiltraciónThe remaining solids were filtered off
  4. 4
    Concentraciónthe filtrate was concentrated

Procedimiento

To a stirring mixture of lithium aluminum hydride (2.22 g, 58.5 mmol) in tetrahydrofuran (70 mL) was added compound 399 (3.60 g, 13.8 mmol), portionwise over three minutes. After 1.25 hours of reflux the reaction was cooled to room temperature and quenched with water (2.22 mL), then 1N NaOH (2.22 mL), then water (2×2.22 mL). The remaining solids were filtered off, and the filtrate was concentrated to give compound 402 (2.81 g, 82%). LCMS-ESI (POS), M/Z, M+1: Found 247.1, Calculated 247.2.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08841312B2uspto-grants-2014_09