Реакция #87404

ord-46c754c58ea941b6a092d2ed98a61f48

Растворители

Условия реакции

Температура
0°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураThe reaction mixture was refluxed for 16 h
  2. 2
    КонцентрированиеThe mixture was concentrated in vacuo and hydrochloric acid (aq, 10%)
  3. 3
    workup.ADDITIONwas added
  4. 4
    ДругоеThe precipitate was isolated by filtration
  5. 5
    Другоеdried

Методика

6-[(Cyclopropylmethoxy)methyl]-2-sulfanylidene-1,2,3,4-tetrahydropyrimidin-4-one (10.3 g, 48.5 mmol) was added to bromoacetic acid (21.5 g, 155 mmol, 3.2 eq) in EtOH (108 mL) and H2O (441 mL). The reaction mixture was refluxed for 16 h then cooled down to rt and basified to pH˜10 with sodium hydroxide (3 M, aq). The mixture was concentrated in vacuo and hydrochloric acid (aq, 10%) was added. The mixture was cooled to 0° C. The precipitate was isolated by filtration and dried to give the title compound as a solid (3.5 g, 37%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09439904B2uspto-grants-2016_09