Phosphorus oxychloride → 4,7-Dichloropyrido[3,2-d]pyrimidine

HRID 1526558노트

반응식

HRID 1526558 반응식
[Cl:1][C:2]1[CH:11]=[N:10][C:9]2[C:8](=O)[N:7]=[CH:6][NH:5][C:4]=2[CH:3]=1.CCN(C(C)C)C(C)C.P(Cl)(Cl)([Cl:24])=O>C1(C)C=CC=CC=1>[Cl:24][C:8]1[C:9]2[N:10]=[CH:11][C:2]([Cl:1])=[CH:3][C:4]=2[N:5]=[CH:6][N:7]=1

참가 물질

5

반응물 3

HCID 24813Phosphorus oxychlorideHCID 81531DiisopropylethylamineHCID 1785182197-chloro-1H-pyrido[3,2-d]pyrimidin-4-one

생성물 1

HCID 714284454,7-Dichloropyrido[3,2-d]pyrimidine

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a mixture of 7-chloropyrido[3,2-d]pyrimidin-4(1H)-one (250 mg, 1.377 mmol) in toluene (12 mL) were added DIPEA (0.73 mL, 4.20 mmol) and phosphorus oxychloride (0.391 mL, 4.27 mmol), and the reaction was stirred at reflux for 1 hour. After cooling to RT, the reaction mixture was concentrated to provide the title compound. LC/MS (ESI+) m/z=200 (M+H)+.

후처리

  1. temperatureat reflux for 1 hour
  2. concentrationthe reaction mixture was concentrated

출처 및 근거

ORD 기록
ord-e0b1df88ef4e49cb9c77cec41a178fc8
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09085576B2

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