Water → 139393-89-8

HRID 1032996

反応式

HRID 1032996 の反応式
[C:1]([C:3]1[C:4](=O)[NH:5][C:6]([CH3:11])=[C:7]([CH2:9][CH3:10])[CH:8]=1)#[N:2].P(Cl)(Cl)(Cl)(Cl)[Cl:14].O>CCCCCC>[Cl:14][C:4]1[C:3]([C:1]#[N:2])=[CH:8][C:7]([CH2:9][CH3:10])=[C:6]([CH3:11])[N:5]=1

参加物

5

反応物 3

HCID 962WaterHCID 24819Phosphorus pentachlorideHCID 102411095-Ethyl-6-methyl-2-oxo-1,2-dihydropyridine-3-carbonitrile

生成物 1

HCID 10103778139393-89-8収率 61.2%

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

実験手順

3-Cyano-5-ethyl-6-methyl-2-(1H)-pyridinone (22.9 g, 0.141 mol) and phosphorus pentachloride (33.1 g, 0.159 mol) were intimately mixed and heated at 110°-120° C. for one hour. The liquified solids were poured onto crushed ice and water and the semi-solid was extracted into chloroform. This extract was washed with water, saturated aqueous NaHCO3, dried (Na2SO4), filtered and evaporated. This amber oil was dissolved in hexane and the insoluble material was removed when filtered through a pad of charcoal. Removal of the solvent gave a light yellow oil which solidified (17.7 g). Trituration of this solid with cold hexane yielded 15.6 g (61%) of pure product, m.p. 63°-64° C.

後処理

  1. temperatureheated at 110°-120° C. for one hour
  2. additionThe liquified solids were poured
  3. extractionthe semi-solid was extracted into chloroform
  4. washThis extract was washed with water, saturated aqueous NaHCO3
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. customevaporated
  8. dissolutionThis amber oil was dissolved in hexane
  9. customthe insoluble material was removed when
  10. filtrationfiltered through a pad of charcoal
  11. customRemoval of the solvent
  12. customgave a light yellow oil which

出典と根拠

ORDレコード
ord-e6188d38ad184fbca495cc27327452eb
出典データセット
uspto-grants-1994_05
特許番号
US05308854

関連ノート

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