反応 #447164

ord-51506be5026a44eab947d441bad614c7

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The resulting mixture was heated
  2. 2
    温度at reflux for 16 hours
  3. 3
    温度The mixture was cooled
  4. 4
    ろ過filtered
  5. 5
    洗浄The solid was washed with tetrahydrofuran
  6. 6
    乾燥the filtrate was dried with anhydrous magnesium sulfate
  7. 7
    ろ過filtered
  8. 8
    その他The filtrate was evaporated to dryness

実験手順

To a suspension of 2.5 g of lithium aluminum hydride in 100 ml of anhydrous tetrahydrofuran was added dropwise a solution of 5.0 g of N-[(4-butylphenyl)methyl]5-(trimethylsilyl)pentanamide in tetrahydrofuran. The resulting mixture was heated at reflux for 16 hours. The mixture was cooled, and the complex was decomposed by the cautious portionwise addition of sodium sulfate decahydrate. The mixture was stirred for 1/2 hour and then filtered. The solid was washed with tetrahydrofuran, and the filtrate was dried with anhydrous magnesium sulfate and filtered. The filtrate was evaporated to dryness and gave 4.53 g of the desired product as a colorless liquid, in 95% yield.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05003106uspto-grants-1991_03