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

HRID 930451노트

반응식

HRID 930451 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-aa7383c7f17047ee8217fd130fbad691
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09296734B2

반응 노트

불러오는 중…