Реакция #44525

ord-ee4c67b25ee64efdb3c0893c80b0defa

Уравнение реакции

CSc1nccc(Cl)n1
4-chloro-2-methylsulfanylpyrimidine
N
ammonia
CSc1nccc(N)n1
2-(methylsulfanyl)-4-pyrimidinamine

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураcooled
  2. 2
    Концентрированиеconcentrated
  3. 3
    workup.ADDITIONtreated with water
  4. 4
    Экстракцияextracted with ethyl acetate
  5. 5
    ПромывкаThe extract was washed with brine
  6. 6
    Сушкаdried over anhydrous sodium sulfate
  7. 7
    Концентрированиеconcentrated
  8. 8
    ДругоеThe concentrate was triturated with ethyl ether
  9. 9
    Фильтрацияfiltered

Методика

A mixture of 4-chloro-2-methylsulfanylpyrimidine (8 g) and 7N ammonia in methanol (100 mL) at 100° C. was stirred for 2 days in a sealed tube, cooled, concentrated, treated with water, and extracted with ethyl acetate. The extract was washed with brine, dried over anhydrous sodium sulfate, and concentrated. The concentrate was triturated with ethyl ether and filtered. 1H NMR (300 MHz, CDCl3) δ 8.06 (d, 1H), 6.12 (d, 1H), 4.83 (s, 2H), 2.51 (s, 3H).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07737159B2uspto-grants-2010_06