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

HRID 2417671노트

반응식

HRID 2417671 반응식
[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

참가 물질

4

반응물 2

HCID 24819Phosphorus pentachlorideHCID 178433984HCID 178433984, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 24813Phosphorus oxychloride용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-93e5149f6ab841788b93b07fb3b08038
출처 데이터셋
uspto-grants-1984_09
특허 번호
US04469868

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