Phosphorus oxychloride → HCID 22756855, 화합물

HRID 65988노트

반응식

HRID 65988 반응식
[CH3:1][N:2]1[CH:10]=[C:9]2[C:4]([N:5]=[C:6]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH:7]=[C:8]2O)=[N:3]1.P(Cl)(Cl)([Cl:20])=O>>[Cl:20][C:8]1[C:9]2[C:4](=[N:3][N:2]([CH3:1])[CH:10]=2)[N:5]=[C:6]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH:7]=1

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 178479971HCID 178479971, 화합물

생성물 1

HCID 22756855HCID 22756855, 화합물

실험 절차

39 g. of 2-methyl-6-phenyl-2H-pyrazolo[3,4-b]pyridin-4-ol (0.17 mol.) are refluxed in 195 ml. of phosphorus oxychloride for 90 minutes. The excess phosphorus oxychloride is removed in vacuo and the residue is poured onto ice. Concentrated aqueous ammonia is added under external cooling to adjust the mixture to pH 8-9. Stirring is continued for one additional hour. The collected 4-chloro-2-methyl-6-phenyl-2H-pyrazolo[3,4-b]pyridine is washed with water and dried at 70°, yield: 41 g. (100%); m.p. 177°-179°. Recrystallization from ethyl acetate gives a melting point of 189°-190°.

후처리

  1. customThe excess phosphorus oxychloride is removed in vacuo
  2. additionthe residue is poured onto ice
  3. additionConcentrated aqueous ammonia is added
  4. temperatureunder external cooling
  5. washThe collected 4-chloro-2-methyl-6-phenyl-2H-pyrazolo[3,4-b]pyridine is washed with water
  6. customdried at 70°
  7. customRecrystallization from ethyl acetate
  8. customgives a melting point of 189°-190°

출처 및 근거

ORD 기록
ord-519c1d9a9cdc4c52b19f56652c347634
출처 데이터셋
uspto-grants-1978_12
특허 번호
US04129738

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