반응 #2063062

ord-2bfd6f20858c4c52bd650b3af0c2c4bc

반응 방정식

NCCN1CCN(c2ccc(Cl)c(Cl)c2)CC1
4-(3,4-dichlorophenyl)-1-piperazineethanamine
Cc1ccc(N=C=S)cc1
4-methyl-1-isothiocyanatobenzene
Cc1ccc(NC(=S)NCCN2CCN(c3ccc(Cl)c(Cl)c3)CC2)cc1
N-(4-methylphenyl)-N′-[2-[4-(3,4-dichlorophenyl)-1-piperazinyl]ethyl]thiourea
수율 99.2%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The solvent was evaporated
  2. 2
    기타The residue was recrystallized from DIPE
  3. 3
    여과The precipitate was filtered off
  4. 4
    기타dried
  5. 5
    기타The product was used without further purification

실험 절차

A mixture of 4-(3,4-dichlorophenyl)-1-piperazineethanamine (0.01 mol) and 4-methyl-1-isothiocyanatobenzene (0.01 mol) in tetrahydrofuran (300 ml) was stirred at room temperature for 1 hour. The solvent was evaporated. The residue was recrystallized from DIPE. The precipitate was filtered off and dried. The product was used without further purification, yielding 4.2 g N-(4-methylphenyl)-N′-[2-[4-(3,4-dichlorophenyl)-1-piperazinyl]ethyl]thiourea (interm. 6).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06224849B1uspto-grants-2001_05