تفاعل #166413

ord-ab295fc97e9f47a881009d73c7510aad

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةAfter 1.25 hours of reflux the reaction
  2. 2
    أخرىquenched with water (2.22 mL)
  3. 3
    ترشيحThe remaining solids were filtered off
  4. 4
    تركيزthe filtrate was concentrated

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08841312B2uspto-grants-2014_09