Реакция #69650

ord-d824fdad02994a7592fb6dcf0c2d1703

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ФильтрацияAfter uptake of H2 (3 equiv; 0.0015 mol), the catalyst was filtered off
  2. 2
    Концентрированиеthe filtrate was concentrated by rotary evaporation
  3. 3
    Другоеdried in vacuo over 16 hours at 40° C.

Методика

A mixture of 4-[[4-(4-cyano-2,6-dimethylphenoxy)-5-nitro-2-pyrimidinyl]amino]benzonitrile (0.0005 mol) in tetrahydrofuran (20 ml) was hydrogenated overnight with Pd/C 10% (0.100 g) as a catalyst. After uptake of H2 (3 equiv; 0.0015 mol), the catalyst was filtered off and the filtrate was concentrated by rotary evaporation and dried in vacuo over 16 hours at 40° C., yielding 0.15 g of 4-[[5-amino-4-(4-cyano-2,6-dimethylphenoxy)-2-pyrimidinyl]amino]benzonitrile (84%); mp. >300° C. (comp. 50).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08530655B2uspto-grants-2013_09