反応 #4309

ord-53878bc16b5f4166be999b2b304deda7

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04724235uspto-grants-1988_02