Ethyl Acetate → 6-[3-Chloro-4-(ethoxycarbonylmethoxy)phenyl]-4,5-dihydro-3(2H)-pyridazinone

HRID 2072685

反応式

HRID 2072685 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:15](=O)[CH2:16][CH2:17][C:18]([OH:20])=O)[CH:5]=[CH:6][C:7]=1[O:8][CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11].O.[NH2:23][NH2:24].C(OCC)(=O)C>C(O)C>[Cl:1][C:2]1[CH:3]=[C:4]([C:15]2[CH2:16][CH2:17][C:18](=[O:20])[NH:23][N:24]=2)[CH:5]=[CH:6][C:7]=1[O:8][CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11]

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 24654Hydrazine hydrate (1:1)HCID 148782884-[3-Chloro-4-(ethoxycarbonylmethoxy)phenyl]-4-oxobutyric acid

生成物 1

HCID 136876706-[3-Chloro-4-(ethoxycarbonylmethoxy)phenyl]-4,5-dihydro-3(2H)-pyridazinone

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

1.58 g of 4-[3-chloro-4-(ethoxycarbonylmethoxy)phenyl]-4-oxobutyric acid [prepared as described in step (a) above] was dissolved in 10 ml of ethanol and 0.31 g of 80% v/v aqueous hydrazine hydrate was added thereto, whilst ice-cooling. The mixture was stirred, with ice-cooling, for 5 minutes, and then heated under reflux for 3 hours, after which ethyl acetate was added thereto. The mixture was then cooled to room temperature and the resulting precipitate was recrystallized from a mixture of ethyl acetate and hexane, to give 1.49 g of the title compound, having the same characteristics as the product of Example 1.

後処理

  1. temperaturewhilst ice-cooling
  2. temperaturecooling, for 5 minutes
  3. temperatureheated
  4. temperatureunder reflux for 3 hours
  5. customthe resulting precipitate was recrystallized from a mixture of ethyl acetate and hexane

出典と根拠

ORDレコード
ord-ed0731c1be704990a08d1c7bfffbb9a5
出典データセット
uspto-grants-1990_04
特許番号
US04914093

関連ノート

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