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

HRID 1526550

反応式

HRID 1526550 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 DCM, 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 DCM
  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-6c7a4e1e071b48d9854d192ec089b962
出典データセット
uspto-grants-2015_07
特許番号
US09085576B2

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