Cyanoacetic acid hydrazide → 3-Oxo-5-phenyl-2,3-dihydro-pyridazine-4-carbonitrile

HRID 133016

反応式

HRID 133016 の反応式
[C:1]1([C:7]([CH:9]=O)=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:11]([CH2:13][C:14]([NH:16][NH2:17])=[O:15])#[N:12]>C(O)C>[O:15]=[C:14]1[C:13]([C:11]#[N:12])=[C:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[CH:9]=[N:17][NH:16]1

参加物

4

反応物 2

HCID 8820Cyanoacetic acid hydrazideHCID 14090Phenylglyoxal

生成物 1

HCID 597350963-Oxo-5-phenyl-2,3-dihydro-pyridazine-4-carbonitrile

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Phenyl glyoxal (1.0 g, 7.46 mmol) and cyanoacetohydrazide (740 mg, 7.46 mmol) were heated to reflux in 10 mL ethanol for 16 hours. After cooling, the solvent was evaporated and the crude brown mixture was purified by silica chromatography (1:9 methanol/dichloromethane). The still impure product was further recrystallized from methanol affording 70 mg pure product.

後処理

  1. temperatureAfter cooling
  2. customthe solvent was evaporated
  3. customthe crude brown mixture was purified by silica chromatography (1:9 methanol/dichloromethane)
  4. customThe still impure product was further recrystallized from methanol affording 70 mg pure product

出典と根拠

ORDレコード
ord-5f81c07103d8477b9ab602dbda118848
出典データセット
uspto-grants-2008_06
特許番号
US07390808B2

関連ノート

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