반응 #2897

ord-ea8d9c1fc5de4b569364ab4d8c41abcc

반응 방정식

Cc1ccc(S(=O)(=O)Oc2c(O)cccc2I)cc1
Hydroxy(tosyloxy)iodobenzene
CC(=O)CC(=O)C(F)(F)F
1,1,1-trifluoropentane-2,4-dione
NC(N)=S
thiourea
CC(=O)c1sc(N)nc1C(F)(F)F
title compound
CC(=O)c1sc(N)nc1C(F)(F)F
5-Acetyl-2-amino-4-trifluoromethylthiazole

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The mixture was heated
  2. 2
    온도under reflux for 45 minutes
  3. 3
    온도cooled
  4. 4
    온도The mixture was heated
  5. 5
    온도under reflux for 4 hours
  6. 6
    workup.WAITleft
  7. 7
    기타Evaporation and crystallisation of the residue from dichloromethane

실험 절차

Hydroxy(tosyloxy)iodobenzene (78.5 g) was added to a solution of 1,1,1-trifluoropentane-2,4-dione in acetonitrile (500 ml). The mixture was heated under reflux for 45 minutes, then cooled, and thiourea (15.2 g) was added. The mixture was heated under reflux for 4 hours and then left to stand overnight. Evaporation and crystallisation of the residue from dichloromethane gave the title compound.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05731335uspto-grants-1998_03