反応 #343469

ord-7006f94433194e12989f10dee02a63fa

溶媒

反応条件

温度
16°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度to warm to room temperature
  2. 2
    workup.STIRRINGwas stirred for 1 hour
  3. 3
    workup.STIRRINGthe reaction mixture was stirred at room temperature for 64 hours
  4. 4
    抽出the whole was extracted with methylene chloride
  5. 5
    乾燥The methylene chloride solution was dried
  6. 6
    濃縮concentrated

実験手順

To a chilled solution of 1.12 g (0.0098 mole) of tetrahydrothiophene-3-ol in 15 mL of pyridine was added 1.91 g (0.01 mole) of 4-methylphenylsulfonyl chloride, and the reaction mixture was stirred in the cold, about 16° C., for 1 hour then placed in a cold refrigerator for 16 hours. The reaction mixture was allowed to warm to room temperature and was stirred for 1 hour. An additional 0.3 g (0.0016 mole) of 4-methylphenylsulfonyl chloride was added, and the reaction mixture was stirred at room temperature for 64 hours. The reaction mixture was poured into water, and the whole was extracted with methylene chloride. The methylene chloride solution was dried and concentrated to give 1.28 g of product as an oil.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04702763uspto-grants-1987_10