Sodium Carbonate → 2-chloro-5-phenylnicotinonitrile

HRID 1593666ノート

反応式

HRID 1593666 の反応式
O=[C:2]1[C:7]([C:8]#[N:9])=[CH:6][C:5]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[CH:4][NH:3]1.O=P(Cl)(Cl)[Cl:18].P(Cl)(Cl)(Cl)(Cl)Cl.C(=O)([O-])[O-].[Na+].[Na+]>O>[Cl:18][C:2]1[N:3]=[CH:4][C:5]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[CH:6][C:7]=1[C:8]#[N:9]

参加物

6

反応物 4

HCID 10340Sodium CarbonateHCID 24813Phosphorus oxychlorideHCID 24819Phosphorus pentachlorideHCID 2970612-oxo-5-phenyl-1H-pyridine-3-carbonitrile

生成物 1

HCID 27640432-chloro-5-phenylnicotinonitrile

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

2-Oxo-5-phenyl-1,2-dihydropyridine-3-carbonitrile (2.50 g, 12.7 mmol) was added to a suspension of POCl3 (1.5 ml) and PCl5 (7.35 g) at room temperature. The suspension was then stirred at reflux for 1 hour. The reaction mixture was cooled to room temperature and added cautiously to iced water. The solution was then adjusted to pH 11 with sodium carbonate and the resulting white solid was filtered, washed with water, then dried in vacuo to afford the title compound as a solid.

後処理

  1. temperatureat reflux for 1 hour
  2. filtrationthe resulting white solid was filtered
  3. washwashed with water
  4. customdried in vacuo

出典と根拠

ORDレコード
ord-5550bfbf8b014d3b9ea184d4181d7e35
出典データセット
uspto-grants-2007_11
特許番号
US07297792B2

反応ノート

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