Phosphorus pentachloride → 7-Chloro-1,3,5-trimethyl-1H-pyrazolo[4,3-d]pyrimidine

HRID 2417659ノート

反応式

HRID 2417659 の反応式
[CH3:1][N:2]1[C:10]2[C:9](O)=[N:8][C:7]([CH3:12])=[N:6][C:5]=2[C:4]([CH3:13])=[N:3]1.P(Cl)(Cl)(Cl)(Cl)[Cl:15]>P(Cl)(Cl)(Cl)=O>[Cl:15][C:9]1[C:10]2[N:2]([CH3:1])[N:3]=[C:4]([CH3:13])[C:5]=2[N:6]=[C:7]([CH3:12])[N:8]=1

参加物

4

反応物 2

HCID 24819Phosphorus pentachlorideHCID 178433418HCID 178433418、化合物

生成物 1

HCID 133384077-Chloro-1,3,5-trimethyl-1H-pyrazolo[4,3-d]pyrimidine収率 98%

試薬・触媒・溶媒 1

HCID 24813Phosphorus oxychloride溶媒

実験手順

A mixture of 30.5 g (0.17 mol) of 1,3,5-trimethyl-1H-pyrazolo[4,3-d]pyrimidin-7-ol and 37 g (0.18 mol) of phosphorus pentachloride in 350 ml of phosphorus oxychloride is stirred under reflux for seven hours and the resulting solution is evaporated in vacuo. The solid residue is redissolved in 300 ml of methylenedichloride and stirred with 200 ml of a saturated aqueous solution of sodium bicarbonate. The organic layer is dried over MgSO4 and evaporated in vacuo to give 30 g (98%) of 7-chloro-1,3,5-trimethyl-1H-pyrazolo[4,3-d]pyrimidine, mp 91°-93° C. from ethyl acetate-pet ether.

後処理

  1. temperatureunder reflux for seven hours
  2. customthe resulting solution is evaporated in vacuo
  3. dissolutionThe solid residue is redissolved in 300 ml of methylenedichloride
  4. stirringstirred with 200 ml of a saturated aqueous solution of sodium bicarbonate
  5. dry with materialThe organic layer is dried over MgSO4
  6. customevaporated in vacuo

出典と根拠

ORDレコード
ord-b4185639f7834fcd95dd23cbffdf0b11
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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