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

HRID 1952758ノート

反応式

HRID 1952758 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
92.5 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d7907c5139794e55b7b25a26dd08c8f4
出典データセット
uspto-grants-2000_09
特許番号
US06114334

反応ノート

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