Phosphorus oxychloride → 2,5-Dichloropyrido[3,4-b]pyrazine

HRID 627611

反応式

HRID 627611 の反応式
[Cl:1][C:2]1[C:7]2[N:8]=[CH:9][C:10](=O)[NH:11][C:6]=2[CH:5]=[CH:4][N:3]=1.P(Cl)(Cl)([Cl:15])=O>>[Cl:15][C:10]1[N:11]=[C:6]2[CH:5]=[CH:4][N:3]=[C:2]([Cl:1])[C:7]2=[N:8][CH:9]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 867157425-Chloropyrido[3,4-b]pyrazin-2(1H)-one

生成物 1

HCID 867157432,5-Dichloropyrido[3,4-b]pyrazine収率 92.4%

反応条件

温度
110 °C

実験手順

A suspension of 5-chloropyrido[3,4-b]pyrazin-2(1H)-one (0.57 g, 3.14 mmol) in phosphorus oxychloride (10.24 mL, 110 mmol) was stirred at 110° C. for two hours, and then concentrated. The residue was dissolved in dichloromethane, washed with saturated sodium bicarbonate, dried over anhydrous sodium sulfate, filtered, and concentrated to afford the title compound (580 mg, 2.90 mmol). MS m/z=200 (M+H).

後処理

  1. concentrationconcentrated
  2. dissolutionThe residue was dissolved in dichloromethane
  3. washwashed with saturated sodium bicarbonate
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-fbce1ab24e0542149d7b3ac2d894b99b
出典データセット
uspto-grants-2016_04
特許番号
US09309263B2

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