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

HRID 1833344노트

반응식

HRID 1833344 반응식
[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

참가 물질

3

반응물 2

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

생성물 1

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

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-7e2fc4a868fb42398ae8234a58fe9b1c
출처 데이터셋
uspto-grants-1978_01
특허 번호
US04066645

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