Реакция #47847

ord-03422f858edf4ef7aae928893ffd282e

Реагенты

Нет

Растворители

Условия реакции

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

Обработка

  1. 1
    workup.STIRRINGThe resulting mixture was stirred at RT overnight
  2. 2
    ДругоеSeparated the layers
  3. 3
    Экстракцияthe aqueous layer was extracted with EtOAc (3×300 mL)
  4. 4
    Промывкаwashed with brine (2×300 mL)
  5. 5
    Сушкаdried over MgSO4
  6. 6
    Фильтрацияfiltered
  7. 7
    Концентрированиеconcentrated
  8. 8
    Другоеto give (33 g)

Методика

To 1 L round-bottom flask was added 4-chloro-2-(methylthio)thieno[2,3-d]pyrimidine (35.0 g, 162 mmol), THF (300 mL). The solution was stirred at 0° C. and treated dropwise with a solution of OXONE (209 g, 339 mmol) in water (350 mL). The resulting mixture was stirred at RT overnight. The reaction mixture was diluted with EtOAc (500 mL) and water (300 mL). Separated the layers, the aqueous layer was extracted with EtOAc (3×300 mL). Organic layers were combined, washed with brine (2×300 mL), dried over MgSO4, filtered and concentrated to give (33 g). MS (ES+): 249 (M+H)+.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07745449B2uspto-grants-2010_06