Реакция #62077

ord-a98757de6faa4031934c2f85cda29302

Растворители

Условия реакции

Температура
60°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ЭкстракцияThe mixture was then extracted
  2. 2
    СушкаThe combined organics were dried (MgSO4)
  3. 3
    Фильтрацияfiltered
  4. 4
    Концентрированиеconcentrated in vacuo

Методика

To a solution of 2-(4-Hydroxy-thianthren-1-yl)-6-morpholin-4-yl-pyran-4-one (130) (1.20 g, 2.91 mmol) in dimethylformamide (10 ml), under and inert atmosphere, was added powdered potassium carbonate (1.21 g, 8.75 mmol) and methylbromoacetate (0.55 ml, 5.82 mmol). The temperature of the reaction was raised to 60° C. for 48 hours and then cooled to room temperature before the addition of water (20 mL). The mixture was then extracted using ethyl acetate (3×30 ml). The combined organics were dried (MgSO4), filtered and concentrated in vacuo to give the title compound as an off white solid (1.40 g, 99%) that was suitably clan and required no further purification. m/z (LC-MS, ESP): RT=4.48 min, (M++1)=484

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07429660B2uspto-grants-2008_09