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

HRID 2417659노트

반응식

HRID 2417659 반응식
[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

참가 물질

4

반응물 2

HCID 24819Phosphorus pentachlorideHCID 178433418HCID 178433418, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 24813Phosphorus oxychloride용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b4185639f7834fcd95dd23cbffdf0b11
출처 데이터셋
uspto-grants-1984_09
특허 번호
US04469868

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