반응 #487543

ord-58ee575fb1c44abf9b534308bd2b810c

반응 방정식

FC(F)(F)COc1nc(Cl)nc(Cl)n1
2,4-dichloro-6-(2,2,2-trifluoroethoxy)-1,3,5-triazine
COC(=O)c1ccc(N)cc1OCCCCl
methyl 4-amino-2-(3-chloropropoxy)benzoate
COC(=O)c1ccc(Nc2nc(Cl)nc(OCC(F)(F)F)n2)cc1OCCCCl
methyl 4-(4-chloro-6-(2,2,2-trifluoroethoxy)-1,3,5-triazin-2-ylamino)-2-(3-chloropropoxy)benzoate

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The organic layer was collected
  2. 2
    건조dried over sodium sulfate
  3. 3
    농축concentrated under vacuum
  4. 4
    기타The crude product was purified by silica gel chromatography
  5. 5
    기타The product fractions were collected
  6. 6
    농축concentrated under vacuum

실험 절차

To a solution of 2,4-dichloro-6-(2,2,2-trifluoroethoxy)-1,3,5-triazine (770 mg, 2.79 mmol) in THF (10 mL) was added methyl 4-amino-2-(3-chloropropoxy)benzoate (681 mg, 2.79 mmol) and Hunig'sBase (1.464 mL, 8.38 mmol). The resulting mixture was stirred for 16 h. The reaction was diluted with DCM and water. The organic layer was collected and dried over sodium sulfate, and concentrated under vacuum. The crude product was purified by silica gel chromatography using 20-40% EtOAc/Hexanes. The product fractions were collected and concentrated under vacuum to give methyl 4-(4-chloro-6-(2,2,2-trifluoroethoxy)-1,3,5-triazin-2-ylamino)-2-(3-chloropropoxy)benzoate as a solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08741884B2uspto-grants-2014_06