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

HRID 1833342노트

반응식

HRID 1833342 반응식
[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

참가 물질

3

반응물 2

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

생성물 1

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

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-17fc6805ef334857b62c9c421f655886
출처 데이터셋
uspto-grants-1978_01
특허 번호
US04066645

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