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

HRID 133016

반응식

HRID 133016 반응식
[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

참가 물질

4

반응물 2

HCID 8820Cyanoacetic acid hydrazideHCID 14090Phenylglyoxal

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5f81c07103d8477b9ab602dbda118848
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07390808B2

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