Hydrochloric Acid → Diclomezine

HRID 746274

反応式

HRID 746274 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:10](=O)[CH2:11][CH:12](OC)[C:13]([O:15]C)=O)[CH:5]=[C:6]([Cl:9])[C:7]=1[CH3:8].O.[NH2:21][NH2:22].Cl>CO>[Cl:1][C:2]1[CH:3]=[C:4]([C:10]2[CH:11]=[CH:12][C:13](=[O:15])[NH:21][N:22]=2)[CH:5]=[C:6]([Cl:9])[C:7]=1[CH3:8]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 24654Hydrazine hydrate (1:1)HCID 23310759HCID 23310759、化合物

生成物 1

HCID 93341Diclomezine収率 70.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 3.05 g (0.01 mole) of methyl 4-(3,5-dichloro-4-methylphenyl)-2-methoxy-4-oxobutyrate, 0.6 g (0.012 mole) of hydrazine monohydrate and 30 ml of methanol was heated under reflux for 3.5 hours. 1.1 ml of concentrated hydrochloric acid was then added to the mixture, after which it was again heated under reflux for a further 6 hours. At the end of this time, the solvent was distilled off and the residue was washed, in turn, with water and with a small amount of diethyl ether, after which it was dried to give 1.80 g of the desired product. The washings were extracted with ethyl acetate and the extract was dried over anhydrous sodium sulphate, after which the organic solvent was distilled off. The residue was washed in turn with benzene and with diethyl ether, to give a further 0.11 g of the desired product. The total yield of 6-(3,5-dichloro-4-methylphenyl)-3(2H)pyridazinone was 1.91 g (74.9%) and the properties of the product were identical with those of the products of Examples 1(d), 2 and 3.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 3.5 hours
  3. temperatureafter which it was again heated
  4. temperatureunder reflux for a further 6 hours
  5. distillationAt the end of this time, the solvent was distilled off
  6. washthe residue was washed, in turn, with water and with a small amount of diethyl ether
  7. customafter which it was dried

出典と根拠

ORDレコード
ord-997ae5c5b2e44e08b77709de0de5c42a
出典データセット
uspto-grants-1986_07
特許番号
US04603201

関連ノート

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