반응 #4691

ord-973abaec5c9e43889008b8fe153c5b7e

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The mixture was filtered
  2. 2
    여과filtered
  3. 3
    기타was dried
  4. 4
    workup.DISSOLUTIONThe product was dissolved in 350 ml of tetrahydrofuran
  5. 5
    여과the solution was filtered
  6. 6
    농축concentrated to a volume of 75 ml
  7. 7
    온도The mixture was cooled
  8. 8
    여과iced and filtered
  9. 9
    세척the recovered product was washed with tetrahydrofuran
  10. 10
    기타dried

실험 절차

2.85 ml of a 6.4N hydrogen chloride solution in ethanol were added to a solution of 5.1 g of the product of Example 6 in 5.1 ml of ethanol and then isopropyl ether was added thereto. The mixture was filtered and the recovered product was empasted several times with isopropyl ether, filtered and was dried. The product was dissolved in 350 ml of tetrahydrofuran and the solution was filtered and concentrated to a volume of 75 ml. The mixture was cooled, iced and filtered and the recovered product was washed with tetrahydrofuran and dried to obtain 3.3 g of 3-ethyl-5-(4-methoxyphenyl)-4-phenyl-4H-1,2,4-triazole hydrochloride melting towards 150° C. with decomposition.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04727084uspto-grants-1988_02