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Urea → 1-(3-Methylphenyl)-3,4-dihydropyrido[2,3-d]pyrimidin-2(1H)-one

HRID 436416
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HRID 436416 반응식
[C:1]1([CH3:16])[CH:6]=[CH:5][CH:4]=[C:3]([NH:7][C:8]2[C:13]([CH2:14][NH2:15])=[CH:12][CH:11]=[CH:10][N:9]=2)[CH:2]=1.N[C:18](N)=[O:19]>>[C:1]1([CH3:16])[CH:6]=[CH:5][CH:4]=[C:3]([N:7]2[C:8]3[N:9]=[CH:10][CH:11]=[CH:12][C:13]=3[CH2:14][NH:15][C:18]2=[O:19])[CH:2]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 1176UreaHCID 21452450HCID 21452450, 화합물

생성물 1

HCID 132593341-(3-Methylphenyl)-3,4-dihydropyrido[2,3-d]pyrimidin-2(1H)-one수율 53.9%

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온도
180 °C

실험 절차

To a mixture of 4.3 g 2-(m-toluidino)-3-aminomethylpyridine and 12 g of urea was heated at 180° C for 2 hours and further heated at 200° C for 30 minutes. After cooling, crude reaction product precipitated was collected by filtration and washed with sufficient amounts of warm water. This product was purified by recrystallization from methanol to give 2.6 g of 1-(m-tolyl)-2-oxo-1,2,3,4-tetrahydropyrido[2,3-d]pyrimidine as colorless prisms, melting at 212° - 214° C.

후처리

  1. temperaturefurther heated at 200° C for 30 minutes
  • temperatureAfter cooling
  • customcrude reaction product
  • customprecipitated
  • filtrationwas collected by filtration
  • washwashed with sufficient amounts of warm water
  • customThis product was purified by recrystallization from methanol
  • 출처 및 근거

    ORD 기록
    ord-0bc6a1ed3c6b4551b6bb5f4cc2e14fe4
    출처 데이터셋
    uspto-grants-1977_02
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04009166

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