Phosphorus oxychloride → 5,7-Dichloro-[1,2,4]triazolo[1,5-c]pyrimidine

HRID 2389766노트

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HRID 2389766 반응식
[Cl:1][C:2]1[N:7]=[C:6](O)[N:5]2[N:9]=[CH:10][N:11]=[C:4]2[CH:3]=1.P(Cl)(Cl)([Cl:14])=O>>[Cl:14][C:6]1[N:5]2[N:9]=[CH:10][N:11]=[C:4]2[CH:3]=[C:2]([Cl:1])[N:7]=1

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 178517804HCID 178517804, 화합물

생성물 1

HCID 552791785,7-Dichloro-[1,2,4]triazolo[1,5-c]pyrimidine

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온도
120 °C

실험 절차

927 mg (4.19 mmol) of 7-chloro[1,2,4]triazolo[1,5-c]pyrimidin-5-ol (Example 52A) are suspended in 16.9 g (110.13 mmol) of phosphoryl chloride under argon and heated at 120° C. for 4 h. After this time, the excess phosphoryl chloride is removed in vacuo, and the residue is distilled together with toluene. The residue is suspended in water, the pH is brought to 7 with saturated aqueous sodium bicarbonate solution, and the precipitated solid is filtered off with suction. The latter is washed with water and dried over phosphorus pentoxide for 18 h. 389 mg (49% of theory) of the product are obtained.

후처리

  1. customAfter this time, the excess phosphoryl chloride is removed in vacuo
  2. distillationthe residue is distilled together with toluene
  3. filtrationthe precipitated solid is filtered off with suction
  4. washThe latter is washed with water
  5. dry with materialdried over phosphorus pentoxide for 18 h
  6. custom389 mg (49% of theory) of the product are obtained

출처 및 근거

ORD 기록
ord-a4b39178bc684441afe6712af9b378e3
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08273752B2

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