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

HRID 1833342ノート

反応式

HRID 1833342 の反応式
[CH3:1][C:2]1[CH:15]=[C:5]2[NH:6][C:7](=O)[C:8]3[CH:13]=[N:12][CH:11]=[CH:10][C:9]=3[N:4]2[N:3]=1.P(Cl)(Cl)([Cl:18])=O>>[Cl:18][C:7]1[C:8]2[CH:13]=[N:12][CH:11]=[CH:10][C:9]=2[N:4]2[N:3]=[C:2]([CH3:1])[CH:15]=[C:5]2[N:6]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 1361423592-Methylpyrazolo[1,5-a]pyrido[3,4-e]pyrimidin-5(4H)-one

生成物 1

HCID 213891855-Chloro-2-methylpyrazolo[1,5-a]pyrido[3,4-e]pyrimidine

実験手順

200 g. of 2-methylpyrazolo[1,5-a]pyrido[3,4-e]-pyrimidin-5(4H)-one of Example 1c are refluxed with 800 ml. of phosphorus oxychloride overnight. The excess phosphorus oxychloride is removed in vacuo and the oily residue decomposed by pouring on ice. The acidic aqueous solution is made alkaline with sodium hydroxide. The precipitated 5-chloro-2-methylpyrazolo[1,5-a]pyrido[3,4-e]pyrimidine is filtered off, yield: 143 g. (66%); m.p. 169.8° (ethyl acetate).

後処理

  1. customThe excess phosphorus oxychloride is removed in vacuo
  2. additionby pouring on ice
  3. filtrationThe precipitated 5-chloro-2-methylpyrazolo[1,5-a]pyrido[3,4-e]pyrimidine is filtered off

出典と根拠

ORDレコード
ord-17fc6805ef334857b62c9c421f655886
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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