تفاعل #11963

ord-2bfa4290bd144e32ab8ac973d4d7ed90

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزthe reaction solution was concentrated
  2. 2
    workup.DISTILLATIONazeotropically distilled with methanol
  3. 3
    أخرىThe residue was purified by silica gel column chromatography (1 g, chloroform/methanol/water=7/3/0.5)

الإجراء التجريبي

The compound obtained in Example 53-3 (19.0 mg) was dissolved in methanol (0.19 ml) and 4 mol/l hydrochloric acid/dioxane (0.19 ml) was added. After 2.5 hours, the reaction solution was concentrated and azeotropically distilled with methanol. The residue was purified by silica gel column chromatography (1 g, chloroform/methanol/water=7/3/0.5). The obtained title compound was dissolved in methanol. Activated carbon (4 mg) was added to the solution, followed by filtration and concentration. After the addition of 1 mol/l hydrochloric acid and a small amount of methanol, the residue was concentrated and dried under reduced pressure to obtain hydrochloride of the title compound (17.9 mg) as a yellow solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07098215B2uspto-grants-2006_08