Diethyl Malonate → Sbb038952

HRID 1076644

반응식

HRID 1076644 반응식
[Na].[CH2:2]([NH:6][C:7]([NH2:9])=[O:8])[CH2:3][CH2:4][CH3:5].C([O:12][C:13](=O)[CH2:14][C:15](OCC)=[O:16])C>C(O)C>[CH2:2]([N:6]1[C:15](=[O:16])[CH2:14][C:13](=[O:12])[NH:9][C:7]1=[O:8])[CH2:3][CH2:4][CH3:5]

참가 물질

5

반응물 3

HCID 7761Diethyl MalonateHCID 11595ButylureaHCID 5360545Sodium

생성물 1

HCID 4736903Sbb038952수율 68.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 23 g (1 g-atom) sodium metal in 500 ml absolute ethanol were added at room temperature 35 g (0.3 mole) butyl-urea and 48 g (0.3 mole) malonic acid-diethylester. The alcohol was then distilled off in an oil bath held at 120°C and the residue maintained at this temperature for about 16 hours. The residue was then cooled and dissolved in about 300 ml water, stirred with activated carbon and the solution filtered. The clear filtrate was acidified by the addition of concentrated hydrochloric acid to produce 38 g 1-butyl-barbituric acid, representing a yield of 68%. The substance had, after recrystallization from benzene, a melting point of 107°-108°C.

후처리

  1. distillationThe alcohol was then distilled off in an oil bath
  2. customheld at 120°C
  3. temperaturethe residue maintained at this temperature for about 16 hours
  4. temperatureThe residue was then cooled
  5. dissolutiondissolved in about 300 ml water
  6. filtrationthe solution filtered
  7. additionThe clear filtrate was acidified by the addition of concentrated hydrochloric acid

출처 및 근거

ORD 기록
ord-26bb703027e343ba8c4c22f6ea253aca
출처 데이터셋
uspto-grants-1976_05
특허 번호
US03957786

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