HCID 722983, 화합물 → 2-(3-pyridyl)quinazolin-4-one

HRID 1648214노트

반응식

HRID 1648214 반응식
[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

참가 물질

5

반응물 2

HCID 722983HCID 722983, 화합물HCID 10942334Sodium Methoxide

생성물 1

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

시약·촉매·용매 2

HCID 1140Toluene용매HCID 25517Ammonium Chloride용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-24ef03fcfd864c9589c41d0c2b3857c0
출처 데이터셋
uspto-grants-1995_07
특허 번호
US05436233

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