Reaktion #79811

ord-7772a00da23a479dafe8ac3297ba22c8

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe suspension heated briefly
  2. 2
    Sonstigevolatile material was removed under reduced pressure
  3. 3
    SonstigeThe resulting colourless solid was dried to constant weight at 84° C./5 mbar

Vorschrift

trans-7-[3-(4-methylpiperazino)cyclohexyl]-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-4-amine (0.36 g, 0.00075 mol) in 25 ml warm isopropanol was treated with a solution of 0.225 ml 12M hydrochloric acid (0.0027 mol) in 2 ml isopropanol and the suspension heated briefly to boiling then volatile material was removed under reduced pressure. The resulting colourless solid was dried to constant weight at 84° C./5 mbar giving the trans-7-[3-(4-methylpiperazino)cyclohexyl]-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-4-amine tri-hydrochloride (444626) solvated with 1 mol water and 0.25 mol isopropanol (0.25 g, 0.0004 mol) m.p. 304-306° C.(dec).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06713474B2uspto-grants-2004_03