Water → 139393-89-8

HRID 2081530

반응식

HRID 2081530 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 10103778139393-89-8

시약·촉매·용매 1

HCID 8058Hexane용매

실험 절차

3-Cyano-5-ethyl-6-methyl-2-(1H)-pyridinone (22.9 g, .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 pure product, m.p. 63°-64° C.

후처리

  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

출처 및 근거

ORD 기록
ord-6f9963762328474d8a3df7df7c79e040
출처 데이터셋
uspto-grants-1993_02
특허 번호
US05185251

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