Реакция #66680

ord-98b061d40eb0416680b7ea5e231a94a2

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Экстракцияextracted into methylene chloride
  2. 2
    СушкаThe combined eatracts was dried over Na2SO4
  3. 3
    Фильтрацияfiltered
  4. 4
    Концентрированиеconcentrated

Методика

5-[5-Iodo-2-isopropyl-4-(2-trimethylsilanyloxy-ethoxy)-phenoxy]-pyrimidine-2,4-diamine (0.38 g, 0.69 mmol) in a solution of HOAc/THF/H2O in a ratio of 3:1:1.95 ml) was heated at 65° C. for 16 hrs. The pH of the reaction mixture was adjusted to pH=9 and extracted into methylene chloride. The combined eatracts was dried over Na2SO4, filtered and concentrated. Flash chromatography on silica (5% MeOH in methylene chloride with 0.1% NH4OH) gave 2-[4-(2,4-Diamino-pyrimidin-5-yloxy)-2-iodo-5-isopropyl-phenoxy]-ethanol (0.25 g, 86%) as a white solid. (M+H)=431

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08524725B2uspto-grants-2013_09