Benzylurea → 2,4,6(1H,3H,5H)-Pyrimidinetrione, 5-phenyl-1-(phenylmethyl)-

HRID 357072

반응식

HRID 357072 반응식
[CH2:1]([NH:8][C:9]([NH2:11])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:12]1([CH:18]([C:24](OCC)=[O:25])[C:19](OCC)=[O:20])[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.C[O-].[Na+]>CO>[CH2:1]([N:8]1[C:24](=[O:25])[CH:18]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[C:19](=[O:20])[NH:11][C:9]1=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 10853BenzylureaHCID 66514Diethyl phenylmalonateHCID 10942334Sodium Methoxide

생성물 1

HCID 1663402,4,6(1H,3H,5H)-Pyrimidinetrione, 5-phenyl-1-(phenylmethyl)-

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a suspension of 100 g (666 mmol) of benzylurea and 156.8 g (666 mmol) of diethyl phenylmalonate in 340 ml of methanol, 164 ml (666 mmol) of a 4.1M sodium methylate solution was added at room temperature, followed by refluxing for 16 hours. After the reaction mixture was cooled, the solvent was distilled off. After the residue was dissolved in water and insoluble substances were filtered out, the filtrate was adjusted to pH 3-4 by adding concentrated hydrochloric acid. The resulting precipitate was collected by filtration, washed with water and n-hexane-diethyl ether and dried to yield 163.23 g (83.3%, white crystal) of the desired product.

후처리

  1. additionwas added at room temperature
  2. temperatureby refluxing for 16 hours
  3. temperatureAfter the reaction mixture was cooled
  4. distillationthe solvent was distilled off
  5. dissolutionAfter the residue was dissolved in water
  6. filtrationinsoluble substances were filtered out
  7. additionby adding concentrated hydrochloric acid
  8. filtrationThe resulting precipitate was collected by filtration
  9. washwashed with water and n-hexane-diethyl ether
  10. customdried

출처 및 근거

ORD 기록
ord-96ac82532774430d879edb669edb8e8d
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05840732

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