반응 #65693

ord-6cb72450fdfa4b8d8d6fea27607b02ae

용매

반응 조건

온도
110°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도heated to reflux
  2. 2
    기타The separated carboxylic acid sodium salt was removed by filtration
  3. 3
    세척washed with a small amount of ether
  4. 4
    workup.DISSOLUTIONdissolved in 300 ml of water
  5. 5
    온도while cooling with ice
  6. 6
    추출the free carboxylic acid was extracted with ether
  7. 7
    기타the ethereal solution was dried
  8. 8
    기타evaporated

실험 절차

3.74 g of sodium were dissolved in 77 ml of absolute ethanol under argon. The solution was treated dropwise with 25 g of m-bromothiophenol and heated to reflux. Thereafter, 12.4 ml of γ-butyrolactone were added and the reaction mixture was heated to 110° C. for 5 hours. The separated carboxylic acid sodium salt was removed by filtration, washed with a small amount of ether and dissolved in 300 ml of water. The solution was acidified to pH 2 with 1N HCl while cooling with ice, the free carboxylic acid was extracted with ether, the ethereal solution was dried and evaporated. There were obtained 33.1 g of 4-(m-bromophenylmercapto)butyric acid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05420273uspto-grants-1995_05