海萝胶 → 3-ethyl-5-(4-methoxyphenyl)-4-phenyl-4H-1,2,4-triazole hydrochloride

HRID 4595

反应方程式

HRID 4595 反应方程式
[ClH:1].[CH2:2]([C:4]1[N:8]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[C:7]([C:15]2[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][CH:16]=2)=[N:6][N:5]=1)[CH3:3].C(OC(C)C)(C)C>C(O)C>[ClH:1].[CH2:2]([C:4]1[N:8]([C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:7]([C:15]2[CH:16]=[CH:17][C:18]([O:21][CH3:22])=[CH:19][CH:20]=2)=[N:6][N:5]=1)[CH3:3]

参与物

5

反应物 3

HCID 313海萝胶HCID 7914异丙醚HCID 130540223-ethyl-5-(4-methoxyphenyl)-4-phenyl-4H-1,2,4-triazole

产物 1

HCID 201515513-ethyl-5-(4-methoxyphenyl)-4-phenyl-4H-1,2,4-triazole hydrochloride

试剂、催化剂与溶剂 1

HCID 702乙醇溶剂2 次

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.

后处理

  1. filtrationThe mixture was filtered
  2. filtrationfiltered
  3. customwas dried
  4. dissolutionThe product was dissolved in 350 ml of tetrahydrofuran
  5. filtrationthe solution was filtered
  6. concentrationconcentrated to a volume of 75 ml
  7. temperatureThe mixture was cooled
  8. filtrationiced and filtered
  9. washthe recovered product was washed with tetrahydrofuran
  10. customdried

来源与证据

ORD记录
ord-973abaec5c9e43889008b8fe153c5b7e
来源数据集
uspto-grants-1988_02
专利号
US04727084

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