Реакция #2165229

ord-aa1a95d90d514da6aaffeb2cb7ae06f9

Растворители

Условия реакции

Температура
110°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураthe reaction was cooled to 23° C.
  2. 2
    Фильтрацияfiltered
  3. 3
    ПромывкаThe residue was washed with DCM (150 mL)
  4. 4
    ПромывкаThe residue was subsequently washed with a 10% MeOH/DCM solution (1000 mL)
  5. 5
    КонцентрированиеThe filtrate was concentrated in vacuo

Методика

A solution of 1,1-dimethylethyl N-((4-hydroxy-1,1-dimethyl-2-oxo-6-(trifluoromethyl)-naphthalen-3-yl)carbonyl)glycinate (432 mg, 1045 μmol) in toluene (5 mL), was treated with silica gel (314 mg, 5225 μmol). The reaction was heated at 110° C. After 4 hours, the reaction was cooled to 23° C. and filtered. The residue was washed with DCM (150 mL), and the filtrates were discarded. The residue was subsequently washed with a 10% MeOH/DCM solution (1000 mL). The filtrate was concentrated in vacuo, affording 312 mg of the title compound. MS m/e=358.1 (M+H)+. Calculated for C16H14F3NO5 357.08.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07928139B2uspto-grants-2011_04