Formamide → Pyrido(4,3-d)pyrimidin-4(3H)-one

HRID 1059562

반응식

HRID 1059562 반응식
[NH2:1][C:2]1[C:7]([C:8]([OH:10])=O)=[CH:6][N:5]=[CH:4][CH:3]=1.[CH:11]([NH2:13])=O>>[N:1]1[C:2]2[CH:3]=[CH:4][N:5]=[CH:6][C:7]=2[C:8](=[O:10])[NH:13][CH:11]=1

참가 물질

3

반응물 2

HCID 713FormamideHCID 3199794-Aminonicotinic acid

생성물 1

HCID 135471148Pyrido(4,3-d)pyrimidin-4(3H)-one수율 47%

실험 절차

Crude 4-amino nicotinic acid (2.72 g, 11.4 mmol) in formamide (20 mL) is heated to 170° C. for 12 h. The volatiles are distilled out under reduced pressure (0.8 mmHg). The residual solid is then purified on a medium pressure silica gel column, eluting with 10% MeOH in CHCl3 to give 3H-pyrido[4,3-d]pyrimidin-4-one (780 mg, 47%) as a whitish yellow solid. 1H NMR (DMSO) δ 12.64 (1H, brs), 9.28 (1H, s), 8.83 (1H, d, J=5.5 Hz), 8.30 (1H, s), 7.58 (1H, d, J=5.8 Hz).

후처리

  1. distillationThe volatiles are distilled out under reduced pressure (0.8 mmHg)
  2. customThe residual solid is then purified on a medium pressure silica gel column
  3. washeluting with 10% MeOH in CHCl3

출처 및 근거

ORD 기록
ord-8e7572380b834a62a27cf7327625b916
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06521620B1

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