Water → 5-Methylbarbituric acid

HRID 1251938

반응식

HRID 1251938 반응식
[Na].CO[C:4](=[O:10])[CH:5]([CH3:9])[C:6]([OH:8])=O.[NH2:11][C:12]([NH2:14])=[O:13].O>C(O)C>[CH3:9][CH:5]1[C:4](=[O:10])[NH:14][C:12](=[O:13])[NH:11][C:6]1=[O:8]

참가 물질

6

반응물 4

HCID 962WaterHCID 1176UreaHCID 3006933-Methoxy-2-methyl-3-oxopropanoic acidHCID 5360545Sodium

생성물 1

HCID 2327915-Methylbarbituric acid

시약·촉매·용매 1

HCID 702Ethanol용매3회

실험 절차

46 g (2 mols) of sodium are dissolved in 1 liter of absolute ethanol in a 5-liter flask. To this solution are firstly added 348 g (2 mols) of methyl malonic acid methyl ester; and there is then added dropwise at 70° C. with stirring, within about 5 minutes, a solution of 120 g (2 mols) of urea in 1 liter of absolute ethanol. There is formed a thin suspension, which is diluted with 3.5 liters of ethanol, refluxed for 16 hours and afterwards cooled. There are subsequently added 2 liters of water and, for clearing, a filtering auxiliary (HiFlo) is introduced, and the suspension is filtered. Concentrated hydrochloric acid is then added until a Congo blue colour is indicated, and the mixture is left to stand for several hours in a cool place. A fine white crystalline precipitate is formed, which is filtered and dried. The mother liquor is concentrated by evaporation, diluted with water, and the precipitate is likewise filtered and dried. The crude yield is 263 g of material, which melts at 200°-215° C. After recrystallisation from water, there remain 144 g of white crystals (58% of theory), which melt at 203°-204° C.

후처리

  1. additionand there is then added dropwise at 70° C.
  2. customThere is formed a thin suspension, which
  3. temperaturerefluxed for 16 hours
  4. temperatureafterwards cooled
  5. additionfor clearing, a filtering auxiliary (HiFlo) is introduced
  6. filtrationthe suspension is filtered
  7. additionConcentrated hydrochloric acid is then added until a Congo blue colour
  8. waitthe mixture is left
  9. waitto stand for several hours in a cool place
  10. customA fine white crystalline precipitate is formed
  11. filtrationwhich is filtered
  12. customdried
  13. concentrationThe mother liquor is concentrated by evaporation
  14. additiondiluted with water
  15. filtrationthe precipitate is likewise filtered
  16. customdried
  17. customAfter recrystallisation from water, there
  18. custommelt at 203°-204° C.

출처 및 근거

ORD 기록
ord-4e4b8b2f533d43b08d53b388e425731d
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04741760

연결된 노트

불러오는 중…