反应 #11940

ord-f9b2fbe11f024165adc3b05c701f2695

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他After the reaction
  2. 2
    其他the solvent was removed by distillation
  3. 3
    其他The residue was purified by silica gel column chromatography (1 g, chloroform/methanol/water=7/3/0.5)
  4. 4
    workup.ADDITIONThe obtained product was added with an aqueous solution of hydrochloric acid
  5. 5
    浓缩concentrated
  6. 6
    workup.DISTILLATIONazeotropically distilled with water
  7. 7
    洗涤The resulting solid was washed with ether

实验过程

The compound obtained in Example 11-5 (30.6 mg) was dissolved in methanol (0.7 ml), and 4 mol/l hydrochloric acid/dioxane solution (0.7 ml) was added. The mixture was stirred for 3 hours at room temperature. After the reaction, the solvent was removed by distillation. The residue was purified by silica gel column chromatography (1 g, chloroform/methanol/water=7/3/0.5). The obtained product was added with an aqueous solution of hydrochloric acid, concentrated and then azeotropically distilled with water. The resulting solid was washed with ether to obtain a hydrochloride of the title compound (22.7 mg) as a white solid.

来源

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