تفاعل #11964

ord-7d03949ae1e54900937fdaebc8008d05

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزthe reaction solution was concentrated
  2. 2
    أخرىThe residue was purified by silica gel column chromatography (chloroform/methanol/water=7/3/0.5)
  3. 3
    workup.ADDITIONAfter the addition of 1 mol/l hydrochloric acid
  4. 4
    تركيزthe residue was concentrated
  5. 5
    workup.DISTILLATIONsubjected to azeotropic distillation with methanol

الإجراء التجريبي

The compound obtained in Example 54-3 (7.2 mg) was dissolved in methanol (0.15 ml) and 4 mol/l hydrochloric acid/dioxane solution (0.15 ml) was added. After 2 hours, the reaction solution was concentrated. The residue was purified by silica gel column chromatography (chloroform/methanol/water=7/3/0.5). After the addition of 1 mol/l hydrochloric acid, the residue was concentrated and subjected to azeotropic distillation with methanol to obtain hydrochloride of the title compound (6.3 mg) as a white solid.

المصدر

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