反应 #11964

ord-7d03949ae1e54900937fdaebc8008d05

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    浓缩the reaction solution was concentrated
  2. 2
    其他The 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
    浓缩the residue was concentrated
  5. 5
    workup.DISTILLATIONsubjected to azeotropic distillation with methanol

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07098215B2uspto-grants-2006_08