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

HRID 2417669
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반응식

HRID 2417669 반응식
[CH:1]1([C:4]2[N:5]=[C:6](O)[C:7]3[N:12]([CH3:13])[N:11]=[C:10]([CH3:14])[C:8]=3[N:9]=2)[CH2:3][CH2:2]1.P(Cl)(Cl)(Cl)(Cl)[Cl:17]>P(Cl)(Cl)(Cl)=O>[Cl:17][C:6]1[C:7]2[N:12]([CH3:13])[N:11]=[C:10]([CH3:14])[C:8]=2[N:9]=[C:4]([CH:1]2[CH2:3][CH2:2]2)[N:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24819Phosphorus pentachlorideHCID 178433983HCID 178433983, 화합물

생성물 1

HCID 133384087-Chloro-5-cyclopropyl-1,3-dimethyl-pyrazolo[4,3-d]pyrimidine수율 89.2%

시약·촉매·용매 1

HCID 24813Phosphorus oxychloride용매

실험 절차

A mixture of 5-cyclopropyl-1,3-dimethyl-1H-pyrazolo[4,3-d]pyrimidin-7-ol (14.3 g, 0.07 mol) and 18 g (0.088 mol) phosphorus pentachloride in 150 ml of phosphorus oxychloride is stirred under reflux for seven hours and evaporated in vacuo. The residue is dissolved in methylene dichloride and stirred with a saturated aqueous solution of NaHCO3. The organic layer is separated, dried (MgSO4), and evaporated in vacuo to give 13.9 g (84%) of 7-chloro-5-cyclopropyl-1,3-dimethyl-pyrazolo[4,3-d]pyrimidine, mp 87°-90° C. from heptane.

후처리

  1. temperatureunder reflux for seven hours
  2. customevaporated in vacuo
  3. dissolutionThe residue is dissolved in methylene dichloride
  4. stirringstirred with a saturated aqueous solution of NaHCO3
  5. customThe organic layer is separated
  6. dry with materialdried (MgSO4)
  7. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-7d3910dc38d3422dbdb7eecbb043a7be
출처 데이터셋
uspto-grants-1984_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04469868

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