Hydrazine hydrate (1:1) → N-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenyl)-5-oxopyrazolidine-3-carboxamide

HRID 1641440ノート

反応式

HRID 1641440 の反応式
O.[NH2:2][NH2:3].[Cl:4][C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12](=[O:19])/[CH:13]=[CH:14]/[C:15](OC)=[O:16])=[C:7]([C:20](=[O:27])[NH:21][CH:22]([CH:24]2[CH2:26][CH2:25]2)[CH3:23])[CH:6]=1>C(O)C>[Cl:4][C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12]([CH:13]2[CH2:14][C:15](=[O:16])[NH:3][NH:2]2)=[O:19])=[C:7]([C:20](=[O:27])[NH:21][CH:22]([CH:24]2[CH2:26][CH2:25]2)[CH3:23])[CH:6]=1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 44185603Methyl 4-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenylamino)-4-oxocrotonate

生成物 1

HCID 44185604N-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenyl)-5-oxopyrazolidine-3-carboxamide収率 28.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

A mixed liquid comprising 90 mg of hydrazine monohydrate and 3 ml of ethanol was added to a mixed liquid comprising 0.56 g of methyl 4-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenylamino)-4-oxocrotonate and 3 ml of ethanol, followed by rinsing with 2 ml of ethanol, and reflux under heating for 6 hours. The reaction liquid was stood to cool, the precipitated crystals were subjected to suction filtration, and the obtained crystals were washed with ethanol and air dried to obtain 0.16 g of the desired product (melting point: 248° C.).

後処理

  1. additionwas added to a mixed liquid
  2. washby rinsing with 2 ml of ethanol
  3. temperaturereflux
  4. temperatureunder heating for 6 hours
  5. customThe reaction liquid
  6. temperatureto cool
  7. filtrationthe precipitated crystals were subjected to suction filtration
  8. washthe obtained crystals were washed with ethanol and air
  9. customdried

出典と根拠

ORDレコード
ord-8129bd76f647472bbf94c736d024e31b
出典データセット
uspto-grants-2012_02
特許番号
US08115006B2

反応ノート

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