Phosphorus oxychloride → 5,8-Dichloro-2-methylpyrazolo[1,5-a]pyrido[3,4-e]pyrimidine

HRID 1833344ノート

反応式

HRID 1833344 の反応式
[Cl:1][C:2]1[N:16]=[CH:15][C:5]2[C:6](=O)[NH:7][C:8]3[N:9]([N:10]=[C:11]([CH3:13])[CH:12]=3)[C:4]=2[CH:3]=1.P(Cl)(Cl)([Cl:19])=O>>[Cl:19][C:6]1[C:5]2[CH:15]=[N:16][C:2]([Cl:1])=[CH:3][C:4]=2[N:9]2[N:10]=[C:11]([CH3:13])[CH:12]=[C:8]2[N:7]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 1360252228-chloro-2-methylpyrazolo[1,5-a]pyrido[3,4-e]pyrimidin-5(4H)-one

生成物 1

HCID 213891765,8-Dichloro-2-methylpyrazolo[1,5-a]pyrido[3,4-e]pyrimidine

実験手順

23.5 g. of 8-chloro-2-methylpyrazolo[1,5-a]pyrido[3,4-e]pyrimidin-5(4H)-one of Example 1b are refluxed in 100 ml. of phosphorus oxychloride for 12 hours. The excess phosphorus oxychloride is distilled off in vacuo and the oily residue is poured on ice. After standing for 1 hour, 5,8-dichloro2-methylpyrazolo[1,5-a]pyrido[3,4-e]pyrimidine is filtered off, yield: 17 g. (67%); m.p. 203.4° (ethyl acetate).

後処理

  1. distillationThe excess phosphorus oxychloride is distilled off in vacuo
  2. additionthe oily residue is poured on ice
  3. filtration5,8-dichloro2-methylpyrazolo[1,5-a]pyrido[3,4-e]pyrimidine is filtered off

出典と根拠

ORDレコード
ord-7e2fc4a868fb42398ae8234a58fe9b1c
出典データセット
uspto-grants-1978_01
特許番号
US04066645

反応ノート

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