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

HRID 1526558ノート

反応式

HRID 1526558 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-e0b1df88ef4e49cb9c77cec41a178fc8
出典データセット
uspto-grants-2015_07
特許番号
US09085576B2

反応ノート

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