Phosphorus pentachloride → 1H-Pyrazolo[4,3-d]pyrimidine, 7-chloro-1,3-dimethyl-5-(1-methylethyl)-

HRID 2417671ノート

反応式

HRID 2417671 の反応式
[CH3:1][N:2]1[C:10]2[C:9](O)=[N:8][C:7]([CH:12]([CH3:14])[CH3:13])=[N:6][C:5]=2[C:4]([CH3:15])=[N:3]1.P(Cl)(Cl)(Cl)(Cl)[Cl:17]>P(Cl)(Cl)(Cl)=O>[Cl:17][C:9]1[C:10]2[N:2]([CH3:1])[N:3]=[C:4]([CH3:15])[C:5]=2[N:6]=[C:7]([CH:12]([CH3:14])[CH3:13])[N:8]=1

参加物

4

反応物 2

HCID 24819Phosphorus pentachlorideHCID 178433984HCID 178433984、化合物

生成物 1

HCID 140065561H-Pyrazolo[4,3-d]pyrimidine, 7-chloro-1,3-dimethyl-5-(1-methylethyl)-収率 97.4%

試薬・触媒・溶媒 1

HCID 24813Phosphorus oxychloride溶媒

実験手順

A mixture of 10 g (0.048 mol) of 1,3-dimethyl-5-isopropyl-1H-pyrazolo[4,3-d]pyrimidin-7-ol and 10.2 g (0.049 mol) of phosphorus pentachloride in 70 ml of phosphorus oxychloride is stirred under reflux five hours and evaporated in vacuo. The residue is dissolved in 150 ml of methylene dichloride and stirred with 100 ml of a saturated solution of sodium bicarbonate. The organic layer is separated, dried over MgSO4, and evaporated in vacuo to to give 10.5 g of 7-chloro-1,3-dimethyl-5-isopropyl-1H-pyrazolo[4,3-d]pyrimidine, mp 87°-89° C. from pet ether.

後処理

  1. temperatureunder reflux five hours
  2. customevaporated in vacuo
  3. dissolutionThe residue is dissolved in 150 ml of methylene dichloride
  4. stirringstirred with 100 ml of a saturated solution of sodium bicarbonate
  5. customThe organic layer is separated
  6. dry with materialdried over MgSO4
  7. customevaporated in vacuo

出典と根拠

ORDレコード
ord-93e5149f6ab841788b93b07fb3b08038
出典データセット
uspto-grants-1984_09
特許番号
US04469868

反応ノート

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