Hydrochloric Acid → 4-allyl-5-(3-pyridyl)-1,2,4-triazol-3(2H,4H)-one

HRID 1952758

반응식

HRID 1952758 반응식
[OH-].[Na+].[CH2:3]([NH:6][C:7](=[O:18])[NH:8][NH:9][C:10](=O)[C:11]1[CH:16]=[CH:15][CH:14]=[N:13][CH:12]=1)[CH:4]=[CH2:5].Cl>O>[CH2:3]([N:6]1[C:10]([C:11]2[CH:12]=[N:13][CH:14]=[CH:15][CH:16]=2)=[N:9][NH:8][C:7]1=[O:18])[CH:4]=[CH2:5]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 233000284-Allyl-1-nicotinoylsemicarbazide

생성물 1

HCID 233000014-allyl-5-(3-pyridyl)-1,2,4-triazol-3(2H,4H)-one수율 88.6%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
92.5 °C

실험 절차

1M Aqueous sodium hydroxide solution (175 ml) was added over 10 minutes to a stirred suspension of 4-allyl-1-nicotinoylsemicarbazide (17.2 g) in water (100 ml), then the stirred mixture was heated at 90-95° C. for 17 hours, cooled to ambient temperature, and acidified to pH 5 by the addition of 5M hydrochloric acid. The mixture was concentrated in vacuo, and the resulting solid was collected by filtration and dried in vacuo at ambient temperature to give 4-allyl-5-(3-pyridyl)-1,2,4-triazol-3(2H,4H)-one as an off-white solid (14 g), m.p. 120-125° C.

후처리

  1. temperaturecooled to ambient temperature
  2. concentrationThe mixture was concentrated in vacuo
  3. filtrationthe resulting solid was collected by filtration
  4. customdried in vacuo at ambient temperature

출처 및 근거

ORD 기록
ord-d7907c5139794e55b7b25a26dd08c8f4
출처 데이터셋
uspto-grants-2000_09
특허 번호
US06114334

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