반응 #4309

ord-53878bc16b5f4166be999b2b304deda7

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The solvent is removed by rotary evaporation (vacuum pump)
  2. 2
    기타the residue is partitioned between water (
  3. 3
    workup.ADDITIONpH adjusted to 7 by the addition of dilute hydrochloric acid) and chloroform
  4. 4
    기타The chloroform is removed
  5. 5
    기타The salt is then recrystallized from methanol-diethyl ether

실험 절차

A solution of N-[2-[(4-chlorophenyl)sulfonyl]ethyl]-1-methylethanamine hydrochloride and sodium hydroxide in 500 ml of dimethyl sulfoxide is heated at 95° C. for 2 hrs with stirring. The solvent is removed by rotary evaporation (vacuum pump) and the residue is partitioned between water (pH adjusted to 7 by the addition of dilute hydrochloric acid) and chloroform. The chloroform is removed and the residue is converted to the hydrochloride salt with ethereal hydrogen chloride. The salt is then recrystallized from methanol-diethyl ether to give crystalline title compound.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04724235uspto-grants-1988_02