反応 #65195

ord-0cdd43d2293f4b07afd31b99a9d6e306

反応条件

温度
-78°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The cooling bath is removed
  2. 2
    その他After hydrolysis
  3. 3
    その他the organic phase is separated off
  4. 4
    洗浄the aqueous phase is washed three times with toluene
  5. 5
    洗浄the combined organic phases are washed with saturated sodium chloride solution
  6. 6
    その他dried

実験手順

1.48 g (3.95 mmol) of the compound from Example 5 are dissolved in 30 ml of toluene, the solution is cooled to -78° C. under nitrogen and 6.6 ml (10 mmol) of a 1.5 molar solution of diisobutylaluminium hydride in toluene are added dropwise at this temperature. The cooling bath is removed and the mixture is stirred at room temperature for 2 h. After hydrolysis using 20% strength aqueous potassium sodium tartrate solution, the organic phase is separated off, the aqueous phase is washed three times with toluene, and the combined organic phases are washed with saturated sodium chloride solution and dried using sodium sulphate.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05418243uspto-grants-1995_05