Methylhydrazine → 6-[5-(1-Imidazolylmethyl)-thien-2-yl]-2-methyl-3-oxo-2,3,4,5-tetrahydro-pyridazine

HRID 236275ノート

反応式

HRID 236275 の反応式
[NH:1]1[CH:5]=[CH:4][N:3]=[C:2]1[CH2:6][C:7]1[S:11][C:10]([C:12](=O)[CH2:13][CH2:14][C:15]([OH:17])=O)=[CH:9][CH:8]=1.[CH3:19][NH:20][NH2:21]>O>[NH:3]1[CH:4]=[CH:5][N:1]=[C:2]1[CH2:6][C:7]1[S:11][C:10]([C:12]2[CH2:13][CH2:14][C:15](=[O:17])[N:20]([CH3:19])[N:21]=2)=[CH:9][CH:8]=1

参加物

4

反応物 2

HCID 6061MethylhydrazineHCID 704292984-[5-(1-Imidazolylmethyl)-thien-2-yl]-4-oxobutyric acid

生成物 1

HCID 704292546-[5-(1-Imidazolylmethyl)-thien-2-yl]-2-methyl-3-oxo-2,3,4,5-tetrahydro-pyridazine

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

A mixture of 8.7 g of 4-[5-(1-imidazolylmethyl)-thien-2-yl]-4-oxobutyric acid, 2.9 ml methylhydrazine and 100 ml water was heated at 90° C. for 2 hours. After cooling, the precipitated solid was filtered off, dissolved in chloroform, the chloroform phase washed with dilute caustic soda solution and with water, dried over sodium sulfate and evaporated. The residue was purified by column chromatography (Silica gel//chloroform) and finally recrystallized from ethanol.

後処理

  1. temperatureAfter cooling
  2. filtrationthe precipitated solid was filtered off
  3. dissolutiondissolved in chloroform
  4. washthe chloroform phase washed with dilute caustic soda solution and with water
  5. dry with materialdried over sodium sulfate
  6. customevaporated
  7. customThe residue was purified by column chromatography (Silica gel//chloroform)
  8. customfinally recrystallized from ethanol

出典と根拠

ORDレコード
ord-facaa37b75c84a20a64edf600cdada5b
出典データセット
uspto-grants-1987_02
特許番号
US04643998

反応ノート

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