Tetrahydrofuran → 1-(m-Iodophenyl)-2-oxo-1,2,3,4-tetrahydropyrido[2,3-d]pyrimidine

HRID 436406노트

반응식

HRID 436406 반응식
[I:1][C:2]1[CH:3]=[C:4]([CH:14]=[CH:15][CH:16]=1)[NH:5][C:6]1[C:11]([CH2:12][NH2:13])=[CH:10][CH:9]=[CH:8][N:7]=1.[O:17]1CCC[CH2:18]1>CC(C)=O>[I:1][C:2]1[CH:3]=[C:4]([N:5]2[C:6]3[N:7]=[CH:8][CH:9]=[CH:10][C:11]=3[CH2:12][NH:13][C:18]2=[O:17])[CH:14]=[CH:15][CH:16]=1

참가 물질

4

반응물 2

HCID 8028TetrahydrofuranHCID 21452453HCID 21452453, 화합물

생성물 1

HCID 132593321-(m-Iodophenyl)-2-oxo-1,2,3,4-tetrahydropyrido[2,3-d]pyrimidine

시약·촉매·용매 1

HCID 180Acetone용매2회

실험 절차

To a solution of 3.3 g of 2-(m-iodoanilino)-3-aminomethylpyridine and 30 ml of dry tetrahydrofuran was added 3.2 g of N,N'-carbonyldiimidazole and the mixture was heated under reflux for 12 hours. After the reaction was complete, the solvent was removed from the reaction mixture by distillation under reduced pressure. The residue thus obtained was dissolved in acetone. The acetone solution was placed on a column of alumina and eluted with acetone. The eluate was concentrated and left to yield 2.5 g of 1-(m-iodophenyl)-2-oxo-1,2,3,4-tetrahydropyrido[2,3-d]pyrimidine as colorless needles, melting at 175° - 177° C.

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 12 hours
  3. customthe solvent was removed from the reaction mixture by distillation under reduced pressure
  4. customThe residue thus obtained
  5. washeluted with acetone
  6. concentrationThe eluate was concentrated
  7. waitleft

출처 및 근거

ORD 기록
ord-b160a19d7d28440c84a267054daef3b3
출처 데이터셋
uspto-grants-1977_02
특허 번호
US04009166

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