반응 #55918
ord-e49145092cdf4b1ca864bdd569e42458
반응 방정식
반응 조건
온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도under reflux in a nitrogen atmosphere for 3 hours
- 2세척the aqueous phase washed with chloroform
- 3추출extracted into ether
- 4기타The ether was evaporated off
실험 절차
A solution of ethanethiol (12.6 parts) in dimethyl formamide (60 parts) was added with stirring under nitrogen over a period of 20 minutes to a mixture of sodium hydride (6.6 parts of 80% dispersion in oil) and dry dimethyl formamide (60 parts) cooled to 0° C. After 10 minutes, a solution of 2,3-dihydro-5-methoxy-3,3-dimethylbenzofuran (18 parts) in dimethyl formamide (40 parts) was added and the mixture boiled under reflux in a nitrogen atmosphere for 3 hours. The mixture was then added to water and the aqueous phase washed with chloroform, acidified with hydrochloric acid and extracted into ether. The ether was evaporated off to yield 2,3-dihydro-3,3-dimethyl-benzofuran-5-ol (5.4 parts) as a brown oil.