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

HRID 627611

반응식

HRID 627611 반응식
[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

참가 물질

3

반응물 2

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

생성물 1

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

반응 조건

온도
110 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-fbce1ab24e0542149d7b3ac2d894b99b
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09309263B2

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