反応 #4691

ord-973abaec5c9e43889008b8fe153c5b7e

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過The mixture was filtered
  2. 2
    ろ過filtered
  3. 3
    その他was dried
  4. 4
    workup.DISSOLUTIONThe product was dissolved in 350 ml of tetrahydrofuran
  5. 5
    ろ過the solution was filtered
  6. 6
    濃縮concentrated to a volume of 75 ml
  7. 7
    温度The mixture was cooled
  8. 8
    ろ過iced and filtered
  9. 9
    洗浄the recovered product was washed with tetrahydrofuran
  10. 10
    その他dried

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04727084uspto-grants-1988_02