Phosphorus oxychloride → HCID 178508434、化合物

HRID 1982102ノート

反応式

HRID 1982102 の反応式
[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

参加物

3

反応物 2

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

生成物 1

HCID 178508434HCID 178508434、化合物

反応条件

温度
110 °C

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-b3fd495a34da49408506d66f494a6cc9
出典データセット
uspto-grants-1986_06
特許番号
US04595530

反応ノート

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