HCID 722983、化合物 → 2-(3-pyridyl)quinazolin-4-one

HRID 1648214ノート

反応式

HRID 1648214 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]([NH:9][C:10]2[CH:18]=[CH:17][CH:16]=[CH:15][C:11]=2[C:12]([NH2:14])=[O:13])=O)[CH:2]=1.C[O-].[Na+]>C1(C)C=CC=CC=1.[Cl-].[NH4+]>[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]2[NH:14][C:12](=[O:13])[C:11]3[C:10](=[CH:18][CH:17]=[CH:16][CH:15]=3)[N:9]=2)[CH:2]=1

参加物

5

反応物 2

HCID 722983HCID 722983、化合物HCID 10942334Sodium Methoxide

生成物 1

HCID 1354122732-(3-pyridyl)quinazolin-4-one

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 25517Ammonium Chloride溶媒

実験手順

To a solution of the benzamide compound (11.5 g, prepared in Reference example 6) in 100 mL of toluene was added 95% sodium methoxide (5.7 g). The solution was heated at 60°-80° C. for three hours under nitrogen atmosphere. After cooling to room temperature, the solution was diluted with ammonium chloride solution. After stirring for one-half hour, the mixture was filtered. An NMR of the filtered material indicated the reaction was incomplete. The material was taken up in toluene and ethanol and 95% sodium methoxide (5.7 g) was added. The resulting solution was heated to reflux and stirred via a mechanical stirrer, under nitrogen atmosphere, overnight. The solvent had evaporated and the concentrate in the flask was collected and washed with ammonium chloride solution and methylene chloride. The solid material was collected by filtration and allowed to dry to give the title compound as a gray powder having the following physical data.

後処理

  1. temperatureThe solution was heated at 60°-80° C. for three hours under nitrogen atmosphere
  2. filtrationthe mixture was filtered
  3. additionethanol and 95% sodium methoxide (5.7 g) was added
  4. temperatureThe resulting solution was heated
  5. temperatureto reflux
  6. stirringstirred via a mechanical stirrer, under nitrogen atmosphere, overnight
  7. customThe solvent had evaporated
  8. concentrationthe concentrate in the flask
  9. customwas collected
  10. washwashed with ammonium chloride solution and methylene chloride
  11. filtrationThe solid material was collected by filtration
  12. customto dry

出典と根拠

ORDレコード
ord-24ef03fcfd864c9589c41d0c2b3857c0
出典データセット
uspto-grants-1995_07
特許番号
US05436233

反応ノート

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