Phosphorus oxychloride → HCID 86680708, 화합물

HRID 1500759노트

반응식

HRID 1500759 반응식
[N+:1]([C:4]1[C:5](O)=[N:6][C:7]([C:10]2[CH:11]=[N:12][N:13]3[CH:18]=[CH:17][N:16]=[CH:15][C:14]=23)=[N:8][CH:9]=1)([O-:3])=[O:2].P(Cl)(Cl)([Cl:22])=O>>[Cl:22][C:5]1[C:4]([N+:1]([O-:3])=[O:2])=[CH:9][N:8]=[C:7]([C:10]2[CH:11]=[N:12][N:13]3[CH:18]=[CH:17][N:16]=[CH:15][C:14]=23)[N:6]=1

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 178526803HCID 178526803, 화합물

생성물 1

HCID 86680708HCID 86680708, 화합물수율 86%

반응 조건

온도
90 °C

실험 절차

A suspension of 5-nitro-2-(pyrazolo[1,5-a]pyrazin-3-yl)pyrimidin-4-ol (Preparation 24d, 1.50 g, 5.8 mmol) in phosphoryl trichloride (12 mL) was stirred and heated to 90° C. in a sealed tube. After 2 hours, the mixture was concentrated in vacuo and the residue was azeotroped with toluene. The resultant solid was treated with saturated aqueous sodium hydrogen carbonate solution and, upon scratching, a solid formed which was filtered, washed with water (40 mL) and dried to give the title compound (1.38 g, 86%) as a yellow solid.

후처리

  1. concentrationthe mixture was concentrated in vacuo
  2. customthe residue was azeotroped with toluene
  3. additionThe resultant solid was treated with saturated aqueous sodium hydrogen carbonate solution
  4. customa solid formed which
  5. filtrationwas filtered
  6. washwashed with water (40 mL)
  7. customdried

출처 및 근거

ORD 기록
ord-2b5986abc31b483b89c611ed400a19e9
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09206183B2

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