Реакция #166413

ord-ab295fc97e9f47a881009d73c7510aad

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураAfter 1.25 hours of reflux the reaction
  2. 2
    Другоеquenched with water (2.22 mL)
  3. 3
    ФильтрацияThe remaining solids were filtered off
  4. 4
    Концентрированиеthe filtrate was concentrated

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08841312B2uspto-grants-2014_09