반응 #1372003
ord-5707fad6f3d24a43a92e8f1b456bd42b
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상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타Upon completion of the reaction
- 2농축the mixture was concentrated
- 3workup.ADDITIONA 5% aqueous solution of hydrochloric acid was added to the residue, whereby an oily substance
- 4추출The oily substance was extracted with chloroform
- 5세척washed with a 5% aqueous solution of hydrochloric acid and water in order
- 6농축The extract was concentrated
- 7기타recrystallized from toluene
실험 절차
2,4-Dimethyl-5-(trifluoromethanesulfonamido)benzenesulfonyl chloride (1.5 g) was added to tetrahydrofuran (20 ml) containing propargylamine (0.5 g), and the resultant mixture was allowed to stand overnight at room temperature. Upon completion of the reaction, the mixture was concentrated. A 5% aqueous solution of hydrochloric acid was added to the residue, whereby an oily substance was deposited. The oily substance was extracted with chloroform and washed with a 5% aqueous solution of hydrochloric acid and water in order. The extract was concentrated and recrystallized from toluene to give 1.05 g of N-propargyl-2,4-dimethyl-5-(trifluoromethanesulfonamido)benzenesulfonamide. M.P., 130.5°-132° C.