Lithium iodide → 4-oxo-10-(2-methylpropionamido)-4H-pyrimido[1,2-C]quinazoline-3-carboxylic acid

HRID 1719962ノート

反応式

HRID 1719962 の反応式
[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]

参加物

4

反応物 2

HCID 66321Lithium iodideHCID 13060556methyl 4-oxo-10-(2-methylpropionamido)-4H-pyrimido[1,2-C]quinazoline-3-carboxylate

生成物 1

HCID 130605604-oxo-10-(2-methylpropionamido)-4H-pyrimido[1,2-C]quinazoline-3-carboxylic acid収率 73.1%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
100 °C

実験手順

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).

後処理

  1. temperatureThe reaction mixture was cooled
  2. customto give crystals which
  3. filtrationwere collected by filtration
  4. washwashed with pyridine
  5. customto give yellow crystals, which
  6. customwere separated by filtration
  7. washwashed with water
  8. customdried
  9. washThe crude crystals were washed with a mixture of chloroform and methanol (1:1) two times
  10. customdried

出典と根拠

ORDレコード
ord-ba2d8f206a8c4a0b9e203d8104757f0c
出典データセット
uspto-grants-1985_09
特許番号
US04543356

反応ノート

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