Phosphorus oxychloride → 7-Chloro-1-ethyl-1H-pyrazolo[4,3-d]pyrimidine

HRID 573345노트

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HRID 573345 반응식
[CH2:1]([N:3]1[C:11]2[C:10](O)=[N:9][CH:8]=[N:7][C:6]=2[CH:5]=[N:4]1)[CH3:2].O=P(Cl)(Cl)[Cl:15]>>[Cl:15][C:10]1[C:11]2[N:3]([CH2:1][CH3:2])[N:4]=[CH:5][C:6]=2[N:7]=[CH:8][N:9]=1

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 178463033HCID 178463033, 화합물

생성물 1

HCID 714458087-Chloro-1-ethyl-1H-pyrazolo[4,3-d]pyrimidine

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온도
100 °C

실험 절차

A mixture of 1-ethyl-1H-pyrazolo[4,3-d]pyrimidin-7-ol (2.91 g) and POCl3 (30 mL) was stirred at 100° C. overnight. The mixture was concentrated under reduced pressure. The residue was neutralized with saturated NaHCO3 aqueous solution and extracted with AcOEt. The organic layer was dried over Na2SO4, filtered and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (AcOEt/hexane) to give the title compound (2.14 g).

후처리

  1. concentrationThe mixture was concentrated under reduced pressure
  2. extractionextracted with AcOEt
  3. dry with materialThe organic layer was dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (AcOEt/hexane)

출처 및 근거

ORD 기록
ord-dfa8156422914e4a99cd25b0ab75f904
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09029536B2

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