反応 #93538

ord-2fed1269505b4a02ba1545817fd2479d

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他After completion of the reaction
  2. 2
    洗浄washed with 10% hydrochloric acid, 10% aqueous sodium hydrogen carbonate
  3. 3
    乾燥dried over magnesium sulfate
  4. 4
    workup.DISTILLATIONthe solvent was distilled off
  5. 5
    その他The crude product thus obtained
  6. 6
    その他was purified by a silica gel column chromatography

実験手順

To a solution of 1.5 g of α-mercaptomethyl-β-phenyl-γ-butyrolactone in 30 ml of ethyl ether were added at room temperature 4.3 g of p-n-butylbenzoyl chloride and then 1.9 ml of pyridine. The mixture was kept at room temperature for 2.5 hours. After completion of the reaction, the reaction mixture was diluted with 100 ml of ethyl ether, washed with 10% hydrochloric acid, 10% aqueous sodium hydrogen carbonate and then satureated saline, dried over magnesium sulfate and the solvent was distilled off. The crude product thus obtained was purified by a silica gel column chromatography to give 2.1 g (yield 79%) of the title compound.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04613613uspto-grants-1986_09