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

HRID 627616ノート

反応式

HRID 627616 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-1805bba726ee48d7972ee23fce99471d
出典データセット
uspto-grants-2016_04
特許番号
US09309263B2

反応ノート

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