Phosphorus oxychloride → HCID 178508434, 화합물

HRID 1982102노트

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HRID 1982102 반응식
[NH2:1][C:2]1[N:7]=[C:6]2[N:8]=[CH:9][CH:10]=[C:5]2[C:4](=O)[N:3]=1.P(Cl)(Cl)([Cl:14])=O>>[NH2:1][C:2]1[NH:7][C:6]2=[N:8][CH:9]=[CH:10][C:5]2=[C:4]([Cl:14])[N:3]=1

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 219043482-Amino-4H-pyrrolo[2,3-d]pyrimidin-4-one

생성물 1

HCID 178508434HCID 178508434, 화합물

반응 조건

온도
110 °C

실험 절차

2-Aminopyrrolo[2,3-d]pyrimidin-4-one (45 g) was suspended in phosphorus oxychloride (150 ml) and the suspension was stirred at 110° C. for 3 hours. The excess amount of phosphorus oxychloride was distilled off under reduced pressure and ice water (600 ml) was added to the residue, whereby the residue was thoroughly dissolved. The solution was cooled with stirring and adjusted to pH 9 with concentrated aqueous ammonia. The resulting precipitate was collected by filtration, washed with water and recrystallized from hot methanol (4 l) to give the above-identified compound (34.6 g).

후처리

  1. distillationThe excess amount of phosphorus oxychloride was distilled off under reduced pressure and ice water (600 ml)
  2. additionwas added to the residue, whereby the residue
  3. dissolutionwas thoroughly dissolved
  4. temperatureThe solution was cooled
  5. stirringwith stirring
  6. filtrationThe resulting precipitate was collected by filtration
  7. washwashed with water
  8. customrecrystallized from hot methanol (4 l)

출처 및 근거

ORD 기록
ord-b3fd495a34da49408506d66f494a6cc9
출처 데이터셋
uspto-grants-1986_06
특허 번호
US04595530

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