반응 #81891

ord-f7a16980e13f4fe5801b3bd17ac6f3d2

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도heated
  2. 2
    온도at reflux for 20 min
  3. 3
    기타13 separated as a white powder
  4. 4
    여과This was filtered out
  5. 5
    workup.DISSOLUTIONdissolved in 60 mL of boiling aqueous 75% methanol
  6. 6
    workup.ADDITIONtreated with triethylamine (1.5 mL)
  7. 7
    온도On cooling
  8. 8
    기타off-white flakes separated
  9. 9
    여과Filtration
  10. 10
    기타drying

실험 절차

Compound No. 13: A suspension of 3,5-diacetylaniline (1.95 g) in water (10 mL) was treated with 2-chloro-4,6-diamino-1,3,5-triazine (1.455 g) and concentrated HCl (0.1 mL) and heated at reflux for 20 min. After cooling the hydrochloride of Compound No. 13 separated as a white powder. This was filtered out, dissolved in 60 mL of boiling aqueous 75% methanol and treated with triethylamine (1.5 mL). On cooling, off-white flakes separated. Filtration and drying gave 1.79 g of 2-(3,5-diacetylphenyl)amino-4,6-diamino-1,3,5-triazine, mp 271°-2° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05620983uspto-grants-1997_04