反応 #10590

ord-40e9753b7e624fac9a959e0125d91815

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他(50° C., 2 hours)
  2. 2
    その他the solvent was evaporated under reduced pressure
  3. 3
    workup.ADDITIONThe residue was added with methanol (1 ml) and diethyl ether (3 ml)
  4. 4
    その他The deposited precipitates
  5. 5
    ろ過were collected by filtration
  6. 6
    洗浄washed with diethyl ether

実験手順

According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 6 (249 mg) and 10% hydrogen chloride/methanol solution (5 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with methanol (1 ml) and diethyl ether (3 ml). The deposited precipitates were collected by filtration and washed with diethyl ether to obtain the title compound (188 mg) as white powdery solid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07094789B2uspto-grants-2006_08