1-Aminohomopiperidine → 10-(hexahydro-1H-azepin-1yl)-2,10-dihydroimidazo[1,2-a]pyrido[2,3-d]pyrimidin-5(3H)-one

HRID 2350860ノート

反応式

HRID 2350860 の反応式
Cl[C:2]1[C:7]([C:8]([N:10]2[CH2:14][CH2:13][N:12]=[C:11]2SC)=[O:9])=[CH:6][CH:5]=[CH:4][N:3]=1.[NH2:17][N:18]1[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]1>>[N:18]1([N:17]2[C:2]3[N:3]=[CH:4][CH:5]=[CH:6][C:7]=3[C:8](=[O:9])[N:10]3[CH2:14][CH2:13][N:12]=[C:11]23)[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]1

参加物

3

反応物 2

HCID 221981-AminohomopiperidineHCID 143871351-(2-Chloropyridine-3-carbonyl)-2-methylthio-2-imidazoline

生成物 1

HCID 1438713810-(hexahydro-1H-azepin-1yl)-2,10-dihydroimidazo[1,2-a]pyrido[2,3-d]pyrimidin-5(3H)-one収率 66.3%

反応条件

温度
160 °C

実験手順

A mixture of 10.0 g (39.1 mmoles) of the product of Example 12 and 12.5 g (0.109 mole) of N-aminohomopiperidine was heated at 160° C. for 1 hour. Excess N-aminohomopiperidine was removed by Kugelrohr distillation and the residue was partitioned between methylene chloride and water. The organic layer was dried (sodium sulfate) and concentrated leaving 7.40 g of 10-(hexahydro-1H-azepin-1yl)-2,10-dihydroimidazo[1,2-a]pyrido[2,3-d]pyrimidin-5(3H)-one; melting point 217°-219° C. Total yield 66%.

後処理

  1. customExcess N-aminohomopiperidine was removed by Kugelrohr distillation
  2. customthe residue was partitioned between methylene chloride and water
  3. dry with materialThe organic layer was dried (sodium sulfate)
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-859f62a318fa40cd854cf54ffaa69ebb
出典データセット
uspto-grants-1989_10
特許番号
US04871732

反応ノート

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