반응 #63776

ord-1fa1d906d487453eaed9b357eea79a78

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타Upon completion of the reaction
  2. 2
    농축the mixture was concentrated
  3. 3
    workup.ADDITIONA 5% aqueous solution of hydrochloric acid was added to the residue, whereby an oily substance
  4. 4
    추출The oily substance was extracted with chloroform
  5. 5
    세척washed with a 5% aqueous solution of hydrochloric acid and water in order
  6. 6
    농축The extract was concentrated
  7. 7
    기타recrystallized 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 (Compound No. 35). M.P., 130.5°-132° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04767446uspto-grants-1988_08