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

HRID 4595

반응식

HRID 4595 반응식
[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]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 7914Diisopropyl EtherHCID 130540223-ethyl-5-(4-methoxyphenyl)-4-phenyl-4H-1,2,4-triazole

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매2회

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.

후처리

  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

출처 및 근거

ORD 기록
ord-973abaec5c9e43889008b8fe153c5b7e
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04727084

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