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

HRID 436406ノート

反応式

HRID 436406 の反応式
[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

参加物

4

反応物 2

HCID 8028TetrahydrofuranHCID 21452453HCID 21452453、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b160a19d7d28440c84a267054daef3b3
出典データセット
uspto-grants-1977_02
特許番号
US04009166

反応ノート

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