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Hydrazinium chloride → Diclomezine

HRID 746277
ノート
印刷プレビュー

反応式

HRID 746277 の反応式
Cl[CH:2]([CH2:6][C:7]([C:9]1[CH:14]=[C:13]([Cl:15])[C:12]([CH3:16])=[C:11]([Cl:17])[CH:10]=1)=O)[C:3](O)=[O:4].Cl.[NH2:19][NH2:20]>C(O)C.O>[Cl:17][C:11]1[CH:10]=[C:9]([C:7]2[CH:6]=[CH:2][C:3](=[O:4])[NH:19][N:20]=2)[CH:14]=[C:13]([Cl:15])[C:12]=1[CH3:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 115031Hydrazinium chlorideHCID 134203442-Chloro-4-(3,5-dichloro-4-methylphenyl)-4-oxobutyric acid

生成物 1

HCID 93341Diclomezine収率 66.7%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

1.48 g (0.005 mole) of 2-chloro-4-(3,5-dichloro-4-methylphenyl)-4-oxobutyric acid, prepared as described in step (a) above, were dissolved in a solution of 0.68 g (0.01 mole) of hydrazine hydrochloride in 15 ml of ethanol and 2 ml of water; the solution was then heated under reflux for 3 hours, after which it was cooled. The solvent was then distilled off and 20 ml of water were added to the residue. The mixture was stirred and the resulting crystals were collected by filtration, washed successively with water and with a small amount of diethyl ether and then dried, giving 0.85 g (yield 66.7%) of the desired 6-(3,5-dichloro-4-methylphenyl)-3(2H)pyridazinone, having the same properties as the product obtained in the preceding Examples.

後処理

  1. temperaturethe solution was then heated
  2. temperatureunder reflux for 3 hours
  3. temperatureafter which it was cooled
  4. distillationThe solvent was then distilled off
  5. addition20 ml of water were added to the residue
  6. filtrationthe resulting crystals were collected by filtration
  7. washwashed successively with water and with a small amount of diethyl ether
  8. customdried

出典と根拠

ORDレコード
ord-63e95d34a1f54a31897d064fdc610a45
出典データセット
uspto-grants-1986_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04603201

反応ノート

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