Phosphorus oxychloride → 2,6-Dichloropyrido[3,2-D]pyrimidine
反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[C:10]([N:11]=1)=[CH:9][NH:8][C:7](=O)[N:6]=2.O=P(Cl)(Cl)[Cl:15]>>[Cl:15][C:7]1[N:8]=[CH:9][C:10]2[N:11]=[C:2]([Cl:1])[CH:3]=[CH:4][C:5]=2[N:6]=1参加物
3
実験手順
6-chloro-3H-pyrido[3,2-d]pyrimidin-2-one (3.4 g, 5.2 mmol) are taken up in POCl3 (55 mL) and the mixture is heated for 3 h to 105° C. Then the reaction mixture is added dropwise to ice water, extracted with DCM, the organic phase is dried on MgSO4, the solvent is eliminated in vacuo and 2,6-dichloro-pyrido[3,2-d]pyrimidine (HPLC-MS: MS(M+H)+=200; method AFEC) is obtained.
後処理
- temperaturethe mixture is heated for 3 h to 105° C
- extractionextracted with DCM
- customthe organic phase is dried on MgSO4
出典と根拠
- ORDレコード
- ord-52b7f990777842bab11b671fdc4de15c
- 出典データセット
- uspto-grants-2014_01
- 特許番号
- US08637549B2
反応ノート
読み込み中…