反应 #4691

ord-973abaec5c9e43889008b8fe153c5b7e

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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.

来源

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