Methylhydrazine → 3H-Pyrazol-3-one, 2,4-dihydro-2-methyl-5-phenyl-

HRID 436998ノート

反応式

HRID 436998 の反応式
[C:1]([CH2:9][C:10]([O:12]CC)=O)(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:15][NH:16][NH2:17]>C(O)(C)C>[CH3:15][N:16]1[C:10](=[O:12])[CH2:9][C:1]([C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)=[N:17]1

参加物

4

反応物 2

HCID 6061MethylhydrazineHCID 7170Ethyl benzoylacetate2 回

生成物 1

HCID 1425623H-Pyrazol-3-one, 2,4-dihydro-2-methyl-5-phenyl-

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒2 回

反応条件

温度
20 °C

実験手順

Ethyl benzoylacetate (1,538 g, 8 moles) dissolved in isopropanol (6 l) is placed in a 12 l flask under an atmosphere of nitrogen. Methylhydrazine (410 g, 8.7 moles) in isopropanol (800 ml) is added with stirring in a dropwise manner to the ethyl benzoylacetate solution prewarmed to about 80° C. During the addition external heating is removed. Seeding of the reaction mixture with the product at the point of one-third addition of methylhydrazine causes a copious precipitate of product. This procedure eliminates a large exotherm from occurring at a later stage. After the addition is completed, the reaction mixture is held at about 80° C. for 2 hours. Cooling the slurry to 20° C. and filtering off the solid, a yield of 1,131 g (81%) of product after drying and having a melting point of 211° C. is obtained.

後処理

  1. customis placed in a 12 l flask under an atmosphere of nitrogen
  2. customprewarmed to about 80° C
  3. temperatureDuring the addition external heating
  4. customis removed
  5. additionSeeding of the reaction mixture with the product at the point of one-third addition of methylhydrazine
  6. additionAfter the addition
  7. filtrationfiltering off the solid
  8. dry with materiala yield of 1,131 g (81%) of product after drying
  9. customis obtained

出典と根拠

ORDレコード
ord-e7cdddf26099441cafcd0974c2da747a
出典データセット
uspto-grants-1977_06
特許番号
US04029492

反応ノート

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