반응 #65693
ord-6cb72450fdfa4b8d8d6fea27607b02ae
용매
반응 조건
온도
110°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도heated to reflux
- 2기타The separated carboxylic acid sodium salt was removed by filtration
- 3세척washed with a small amount of ether
- 4workup.DISSOLUTIONdissolved in 300 ml of water
- 5온도while cooling with ice
- 6추출the free carboxylic acid was extracted with ether
- 7기타the ethereal solution was dried
- 8기타evaporated
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.