Phosphorus oxychloride → HCID 86680708、化合物

HRID 1500759ノート

反応式

HRID 1500759 の反応式
[N+:1]([C:4]1[C:5](O)=[N:6][C:7]([C:10]2[CH:11]=[N:12][N:13]3[CH:18]=[CH:17][N:16]=[CH:15][C:14]=23)=[N:8][CH:9]=1)([O-:3])=[O:2].P(Cl)(Cl)([Cl:22])=O>>[Cl:22][C:5]1[C:4]([N+:1]([O-:3])=[O:2])=[CH:9][N:8]=[C:7]([C:10]2[CH:11]=[N:12][N:13]3[CH:18]=[CH:17][N:16]=[CH:15][C:14]=23)[N:6]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 178526803HCID 178526803、化合物

生成物 1

HCID 86680708HCID 86680708、化合物収率 86%

反応条件

温度
90 °C

実験手順

A suspension of 5-nitro-2-(pyrazolo[1,5-a]pyrazin-3-yl)pyrimidin-4-ol (Preparation 24d, 1.50 g, 5.8 mmol) in phosphoryl trichloride (12 mL) was stirred and heated to 90° C. in a sealed tube. After 2 hours, the mixture was concentrated in vacuo and the residue was azeotroped with toluene. The resultant solid was treated with saturated aqueous sodium hydrogen carbonate solution and, upon scratching, a solid formed which was filtered, washed with water (40 mL) and dried to give the title compound (1.38 g, 86%) as a yellow solid.

後処理

  1. concentrationthe mixture was concentrated in vacuo
  2. customthe residue was azeotroped with toluene
  3. additionThe resultant solid was treated with saturated aqueous sodium hydrogen carbonate solution
  4. customa solid formed which
  5. filtrationwas filtered
  6. washwashed with water (40 mL)
  7. customdried

出典と根拠

ORDレコード
ord-2b5986abc31b483b89c611ed400a19e9
出典データセット
uspto-grants-2015_12
特許番号
US09206183B2

反応ノート

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