Cyanoacetamide → 5-Ethyl-6-methyl-2-oxo-1,2-dihydropyridine-3-carbonitrile

HRID 2081529

반응식

HRID 2081529 반응식
[CH2:1]([CH:3]([C:6](=O)[CH3:7])[CH:4]=O)[CH3:2].[Na].[C:10]([CH2:12][C:13]([NH2:15])=[O:14])#[N:11].C([O-])(=O)C.[NH2+]1CCCCC1>O.C(O)(=O)C>[C:10]([C:12]1[C:13](=[O:14])[NH:15][C:1]([CH3:2])=[C:3]([CH2:6][CH3:7])[CH:4]=1)#[N:11]

참가 물질

7

반응물 4

HCID 7898CyanoacetamideHCID 3014295Piperidinium acetateHCID 5360545SodiumHCID 152284102-Ethyl-3-oxobutanal

생성물 1

HCID 102411095-Ethyl-6-methyl-2-oxo-1,2-dihydropyridine-3-carbonitrile

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

실험 절차

According to the method described in J. Heterocyclic Chem., 24, 351 (1987), a mixture of 2-ethyl-3-oxobutanal, sodium salt (37.5 g, 0.275 mmol), cyanoacetamide (25.2 g, 0.30 mol), aqueous piperidinium acetate (22 mL) [prepared from glacial acetic acid (4.2 mL), water (10 mL) and piperidine (7.2 mL)] in water (775 ml) was refluxed for four hours. Glacial acetic acid (30 ml) was added cautiously (much foaming) as the product precipitated. Upon cooling to room temperature, the product was collected by filtration, washed with cold water and air dried. The product had m.p. of 237°-240° C.

후처리

  1. temperaturewas refluxed for four hours
  2. customprecipitated
  3. filtrationthe product was collected by filtration
  4. washwashed with cold water and air
  5. customdried

출처 및 근거

ORD 기록
ord-4cee11361f484c01826e162834fc1fa5
출처 데이터셋
uspto-grants-1993_02
특허 번호
US05185251

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