Реакция #614232

ord-08c09abeeb5c4f1b8c4178503cb53441

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ФильтрацияThe reaction was filtered
  2. 2
    Концентрированиеconcentrated in vacuo
  3. 3
    Другоеpurified by silica gel chromatography (CH2Cl2:20% MeOH in CH2Cl2)

Методика

To a solution of ethyl 2-((3S)-3-(2-chloro-5-fluoropyrimidin-4-ylamino)-1-(nitromethyl)cyclohexyl)ethanoate, 62b, (1.60 g, 4.27 mmol) in MeOH (20 mL) was added Raney Nickel (0.03 g, 0.43 mmol). The reaction was shaken on a Parr apparatus at 40 psi of H2 overnight. The reaction was filtered, concentrated in vacuo and purified by silica gel chromatography (CH2Cl2:20% MeOH in CH2Cl2) to give 155 mg of 62c. LCMS+: 299.13 at 2.87 min (10-90% MeOH, 3/5 grad/run, Formic Acid).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09345708B2uspto-grants-2016_05