Lithium iodide → 4-oxo-10-(2-methylpropionamido)-4H-pyrimido[1,2-C]quinazoline-3-carboxylic acid
반응식
[O:1]=[C:2]1[N:7]2[CH:8]=[N:9][C:10]3[CH:11]=[CH:12][C:13]([NH:16][C:17](=[O:21])[CH:18]([CH3:20])[CH3:19])=[CH:14][C:15]=3[C:6]2=[N:5][CH:4]=[C:3]1[C:22]([O:24]C)=[O:23].[I-].[Li+]>N1C=CC=CC=1>[O:1]=[C:2]1[N:7]2[CH:8]=[N:9][C:10]3[CH:11]=[CH:12][C:13]([NH:16][C:17](=[O:21])[CH:18]([CH3:20])[CH3:19])=[CH:14][C:15]=3[C:6]2=[N:5][CH:4]=[C:3]1[C:22]([OH:24])=[O:23]참가 물질
반응 조건
- 온도
- 100 °C
실험 절차
A mixture of methyl 4-oxo-10-(2-methylpropionamido)-4H-pyrimido[1,2-C]quinazoline-3-carboxylate (5.42 g) and anhydrous lithium iodide (13.55 g) in dry pyridine (54 ml) was stirred at 100° C. for 1.5 hours. The reaction mixture was cooled to give crystals which were collected by filtration and washed with pyridine. The crystals were suspended in water (200 ml). The suspension was adjusted to pH 2.5-3.0 with conc. hydrochloric acid to give yellow crystals, which were separated by filtration, washed with water and dried. The crude crystals were washed with a mixture of chloroform and methanol (1:1) two times and dried. There was obtained crystalline 4-oxo-10-(2-methylpropionamido)-4H-pyrimido[1,2-C]quinazoline-3-carboxylic acid (3.80 g).
후처리
- temperatureThe reaction mixture was cooled
- customto give crystals which
- filtrationwere collected by filtration
- washwashed with pyridine
- customto give yellow crystals, which
- customwere separated by filtration
- washwashed with water
- customdried
- washThe crude crystals were washed with a mixture of chloroform and methanol (1:1) two times
- customdried
출처 및 근거
- ORD 기록
- ord-ba2d8f206a8c4a0b9e203d8104757f0c
- 출처 데이터셋
- uspto-grants-1985_09
- 특허 번호
- US04543356
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