Реакция #60465

ord-f347f953f24d4ebbbb55527545e41df0

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    КонцентрированиеThe separated organic layer was concentrated under reduced pressure
  2. 2
    ДругоеThe resultant residue was purified by NH silica gel column chromatography (ethyl acetate/hexane)

Методика

A mixture of 4-[4-methyl-2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine-1-carboxylic acid t-butyl ester (124 mg, 0.299 mmol) produced in Example (70a), trifluoroacetic acid (1 mL, 12.9 mmol) and dichloromethane (2 mL) was stirred for 2 hours and 30 minutes at room temperature. Saturated aqueous solution of sodium hydrogencarbonate was added to the reaction mixture and extraction was performed with ethyl acetate. The separated organic layer was concentrated under reduced pressure. The resultant residue was purified by NH silica gel column chromatography (ethyl acetate/hexane) to give 85 mg of the title compound as yellow crystals.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07425554B2uspto-grants-2008_09